CN110124629A - A kind of melamine sponge-graphene oxide adsorbent material and its preparation method and application - Google Patents

A kind of melamine sponge-graphene oxide adsorbent material and its preparation method and application Download PDF

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Publication number
CN110124629A
CN110124629A CN201910277857.0A CN201910277857A CN110124629A CN 110124629 A CN110124629 A CN 110124629A CN 201910277857 A CN201910277857 A CN 201910277857A CN 110124629 A CN110124629 A CN 110124629A
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graphene oxide
adsorbent material
sponge
melamine sponge
melamine
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朱锡淼
孙丰强
李晓绵
钟宁宜
黄宇杰
区颖怡
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South China Normal University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
    • 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
    • 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
    • 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
    • C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • 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
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • 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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The purpose of the present invention is to provide a kind of melamine sponge-graphene oxide adsorbent materials and its preparation method and application；Melamine sponge-graphene oxide adsorbent material of the invention has excellent absorption property to the methylene blue dye in water, and the adsorbent material has good hydrophily；To metal cation such as Cu2+、Pb2+、Cd2+Deng there is preferable absorption property, have the characteristics that easily to recycle, reusable, high absorption property, application field is relatively broad；Melamine sponge-graphene oxide adsorbent material preparation method of the invention is simple, based on easy infusion process, by by the compound of melamine sponge and graphene oxide, cost is relatively low, it is easy to produce in enormous quantities, high yield rate, efficiently solves that prepare in graphene oxide composite material that there are operating process in the prior art complicated, the problems such as needing harsh conditions and the equipment such as high temperature and pressure expensive.

Description

A kind of melamine sponge-graphene oxide adsorbent material and preparation method thereof and Using
Technical field
The invention belongs to the technical fields of adsorbent material, and in particular to a kind of melamine sponge-graphene oxide absorption Material and its preparation method and application.
Background technique
Graphene oxide (GO) has two-dimensional planar structure, the pore structure of opening, good flexibility, high machinery strong The features such as degree, chemical property stabilization and large specific surface area；Meanwhile graphene oxide, as a kind of carbon material, surface is contained largely Oxygen-containing group shows good absorption property in terms of wastewater treatment.But graphene oxide composite material is directly applied into water There are still lot of challenges for processing.First, due to the effect of Van der Waals force, be easy to appear between graphene sheet layer it is serious reunion or Superposition, this causes, and surface area is significantly reduced and adsorption capacity declines；Secondly, graphene oxide has good water solubility, It is difficult to be separated from the water out after absorption, can be discharged into environment can bring potential health risk.Develop three-dimensional grapheme material Material such as hydrogel, aeroge are a kind of effective ways to solve the above problems, but prepare three-dimensional grapheme adsorbent material at present That there are operating process is complicated, the problems such as needing the harsh conditions such as high temperature and pressure and needing expensive device.
Redox graphene/sponge composite material exists in the prior art, as patent CN201610123661.2 is public A kind of super-hydrophobic redox graphene/sponge composite material and preparation method has been opened, has been used different from graphite oxide The redox graphene of alkene, the referred to as graphene of redox graphene, most in the prior art is graphene and sponge Composite material, be substantially the adsorbent material of hydrophobic oleophilic oil, graphene oxide and redox graphene are in chemical property It is larger with the diversity ratio in physical property, there is not temporarily related data to disclose at present and is adsorbed with by the sponge for loading graphene oxide The technology of engine dyeing material, and the waste water of organic contamination is adsorbed using graphene oxide merely, not only at high cost, adsorption effect is also not Enough ideals.Therefore, it explores a kind of preparation method easy to operate and easily recycles to obtain, is reusable, high absorption property Three-dimensional porous graphene oxide composite material is particularly important.
Summary of the invention
In view of the above problems, the present invention is based on easy infusion process, by by melamine sponge and graphene oxide It is compound, compared with prior art, cost is relatively low for used reagent material and equipment in operating method by the present invention, and make A kind of composite material with high absorption property is obtained, application field is relatively broad.
The purpose of the present invention is to provide a kind of melamine sponge-graphene oxide adsorbent material and preparation method thereof and Using.
Technical scheme is as follows:
A kind of melamine sponge-graphene oxide adsorbent material, structure are graphene oxide-loaded in melamine sponge Skeleton on, graphene oxide riddles in the hole of melamine sponge.
A kind of application of melamine sponge-graphene oxide adsorbent material, melamine sponge-graphene oxide absorption Material has hydrophily, has excellent absorption property to the methylene blue dye in water, the height applied to organic dye waste water Effect absorption；
It is also applied to the absorption to metal cation, metal cation includes Cu2+、Pb2+、Cd2+。
A kind of preparation method of melamine sponge-graphene oxide adsorbent material, includes the following steps successively to carry out:
1) concentrated sulfuric acid, phosphoric acid and crystalline flake graphite mixing are taken, is stirred evenly；
2) it is slowly added to potassium permanganate, heated at constant temperature and is sufficiently stirred later, obtains mixture A；
3) mixture A temperature after reaction, is down to room temperature；
4) 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；
5) 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；
6) it takes melamine sponge to be pre-processed, is impregnated in graphene oxide solution later and carries out post-processing to get to three Poly cyanamid sponge-graphene oxide adsorbent material；
Wherein, the process for potassium permanganate being added in step 2 can generate faint heat release, during being slowly added to potassium permanganate Its temperature is controlled at 35 DEG C ~ 40 DEG C；
Centrifuge washing described in step 5) include using reagent 5% hydrochloric acid solution；The supernatant liquor of washing to centrifugate can not SO is detected with saturation barium chloride solution4 2-；It is washed with deionized again, until its supernatant liquor can not use the AgNO of 1mol/L3 Solution detects Cl-1；
Pretreatment described in step 6) is 80 DEG C of drying after cleaning melamine sponge with ethyl alcohol；
Post-processing described in step 6) is drying after melamine sponge is filled graphene oxide solution, then sponge is placed in In deionized water, oscillation treatment is carried out, is dried again later to get melamine sponge-graphene oxide adsorbent material.
Beneficial effects of the present invention are as follows:
Melamine sponge-graphene oxide adsorbent material of the invention has excellent suction to the methylene blue dye in water Attached performance, and the adsorbent material has good hydrophily；Adsorbent material of the invention is to metal cation such as Cu2+、Pb2+、Cd2 +Deng there is preferable absorption property, have the characteristics that easily to recycle, reusable, high absorption property；
Melamine sponge-graphene oxide adsorbent material preparation method of the invention is simple, and cost is relatively low, is easy to high-volume Production, high yield rate, efficiently solve that prepare in graphene oxide composite material that there are operating process in the prior art complicated, needs The problems such as harsh conditions such as high temperature and pressure and expensive equipment.
Figure of description
Fig. 1 is the electron-microscope scanning figure of melamine sponge；
Fig. 2 is melamine sponge-graphene oxide composite material electron-microscope scanning figure；
Fig. 3 is the X-ray diffractogram of graphite oxide；
Fig. 4 is the X-ray diffractogram of MS and MS-GO；
Fig. 5 is absorption property figure of the MS and MS-GO to methylene blue solution；
Fig. 6 is the variation diagram for adsorbing methylene blue solution；
Fig. 7 is methylene blue solution absorption property figure of the MS-GO to different pH value.
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
Melamine sponge-graphene oxide adsorbent material the preparation method is as follows:
1) by the dense H of 360mL2SO4With 40mL H3PO4It successively pours into the three neck round bottom of 1L, is slow added into 3.0 G crystalline flake graphite, mechanical stirring is uniform, and control revolving speed is 500 r/min；
2) 18.0 g potassium permanganate under mechanical stirring, are slowly added to set round-bottomed flask after potassium permanganate all adds In 50 DEG C of constant temperature oil baths, 12 h of mechanical stirring；
3) round-bottomed flask after reaction, is taken out, is down to room temperature to it；
4) beaker equipped with 400ml deionized water and 3ml mixed solution of hydrogen peroxide is placed in refrigerator, mixed solution is freezed At 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；
5) it is spent again after the hydrochloric acid solution centrifuge washing (10000 r/min, each 5min) for being 5% by said mixture content Ionized water centrifuge washing；By the graphite oxide freeze-drying after centrifuge washing, solid oxidation graphite is obtained；Accurately weigh 400mg Solid oxidation graphite, by its ultrasonic disperse in 100ml deionized water, then in low speed centrifuge 3000rpm be centrifuged 30min takes supernatant liquor, obtains the graphene oxide solution that concentration is about 4 mg/mL；
6) bulk (2 × 2 × 0.2cm is cut into after cleaning melamine sponge with ethyl alcohol3), 80 DEG C of drying are impregnated in dense later Degree is that the graphene oxide solution of 4 mg/mL takes out sponge block after melamine sponge block is filled graphene oxide solution It is dried at 60 DEG C；The sponge of drying is placed in the deionized water of 50ml again, is shaken in 120rpm, 25 DEG C of constant temperature oscillator Washing 4h is swung, the graphene oxide not being adhered tightly on sponge is removed, is dried at 60 DEG C after sponge is taken out, obtain trimerization Cyanamide sponge-graphene oxide adsorbent material, is denoted as MS-GO；
Fig. 1 is the scanning electron microscope (SEM) photograph of melamine sponge, it can be seen from the figure that being high porosity inside melamine sponge Network structure, skeleton surface is smooth, about 100 microns of aperture, and about 5 microns of skeleton diameter；
Fig. 2 is melamine sponge-graphene oxide composite material scanning electron microscope (SEM) photograph, it can be seen from the figure that graphite oxide Sheet is presented in alkene in the skeleton of melamine sponge, reunites without obvious, and graphene oxide sheet plugs part melamine sea Continuous hole, this is because there are hydrogen bonds between melamine molecule and graphene oxide, since the effect of hydrogen bond is so that oxidation Graphene can be wrapped on sponge skeleton.
Fig. 3 is the X-ray diffractogram of graphite oxide, and Cong Tuzhong spectral line can be seen that, occurs sharp feature at 2 θ=9.6 ° Peak, this illustrates that crystalline flake graphite is substantially completely oxidized to graphite oxide；
Fig. 4 is melamine sponge (MS) and melamine sponge-graphene oxide (MS-GO) X-ray diffractogram；Compared to MS There is a faint characteristic peak at 2 θ=10.0 ° in sample, MS-GO, this explanation is by infusion process in melamine sponge skeleton In loaded graphene oxide, because graphene oxide and melamine sponge interact, the characteristic peak of graphite oxide has compared with Fig. 3 Offset slightly；Because the graphene oxide amount of load is less, therefore the peak at 2 θ=10.0 ° is unobvious；
MS-GO made from melamine sponge MS and embodiment 1 is respectively placed in the Asia that volume is 40ml, concentration is 50mg/L In methyl blue solution, in 25 DEG C, the constant temperature oscillator that revolving speed is 120rpm for 24 hours to methylene blue solution absorption, adsorptivity It can be as shown in Figure 5.
MS-GO made from embodiment 1 is respectively placed in volume is 40ml, concentration is in the methylene blue solution of 50mg/L, With the pH value of hydrochloric acid or sodium hydroxide the adjustment methylene blue solution of 0.1mol/L, shake in 25 DEG C, the constant temperature that revolving speed is 120rpm It swings in device and methylene blue solution is adsorbed for 24 hours, absorption property is as shown in Figure 6.
Fig. 5 is the absorption property figure of melamine sponge and melamine sponge-graphene oxide to methylene blue solution； It is seen that melamine sponge (MS) only has 4.6% to the eliminating rate of absorption of methylene blue, and melamine sponge-oxygen Graphite alkene (MS-GO) up to has 80.7% to the eliminating rate of absorption of methylene blue, and what this had illustrated suction-operated is graphite oxide Alkene, therefore MS-GO is a kind of high-efficiency adsorbent for handling organic dye waste water.
Fig. 6 is the photo of the methylene blue solution color change after different adsorbents adsorb 2min: being followed successively by from left to right 20mg/L methylene blue original solution, the methylene blue solution adsorbed through MS, the methylene blue solution adsorbed through MS-GO；From figure It can be seen that, after MS is adsorbed, methylene blue solution color is almost unchanged；After MS-GO is adsorbed, it is only necessary to pass through 2min, it is sub- Methyl blue solution almost becomes clear, this illustrates that MS-GO has quick, high efficiency of additive capability；In adsorption process, MS-GO is completely submerged in methylene blue solution, illustrates that MS-GO has good hydrophily.
Fig. 7 is methylene blue solution absorption property figure of the MS-GO to different pH value.It is seen that with initial molten The increase of liquid pH, MS-GO increase the eliminating rate of absorption and adsorbance of methylene blue, this is because in acid condition, solution In contain a large amount of H+, the carboxyl and hydroxyl proton that will lead on graphene oxide (GO) turn to-COOH and-OH2+, hydroxyl Protonation can generate electrostatic repulsion, this will inhibit dye of positive ion molecule close to the surface of adsorbent；In higher ph condition Under, H+Concentration is lower, can effectively reduce extra H+Competition with the dye of positive ion to absorption point.In addition, graphene oxide table The carboxyl and hydroxyl in face will form COO and O, enhance the electrostatic attraction between GO and methylene blue molecule, to make to inhale Attached rate and adsorption capacity greatly improve.Because of methylene blue category cationic dyes, the effect between GO mainly passes through electrostatic Attract, therefore, adsorbent material MS-GO of the invention is to metal cation such as Cu2+、Pb2+、Cd2+Deng there is preferable adsorptivity Energy.

Claims (8)

1. a kind of melamine sponge-graphene oxide adsorbent material, which is characterized in that its structure be it is graphene oxide-loaded in On the skeleton of melamine sponge, graphene oxide is riddled in the hole of melamine sponge.
2. a kind of application of melamine sponge-graphene oxide adsorbent material described in claim 1, which is characterized in that three Poly cyanamid sponge-graphene oxide adsorbent material has hydrophily, has excellent adsorptivity to the methylene blue dye in water Can, the efficient absorption applied to organic dye waste water.
3. a kind of application of melamine sponge-graphene oxide adsorbent material described in claim 1, which is characterized in that three Poly cyanamid sponge-graphene oxide adsorbent material is for the absorption to metal cation.
4. a kind of preparation method of melamine sponge-graphene oxide adsorbent material described in claim 1, feature exist In including the following steps successively to carry out:
1) concentrated sulfuric acid, phosphoric acid and crystalline flake graphite mixing are taken, is stirred evenly；
2) it is slowly added to potassium permanganate, heated at constant temperature and is sufficiently stirred later, obtains mixture A；
3) mixture A temperature after reaction, is down to room temperature；
4) 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；
5) 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；
6) melamine sponge after pretreatment, is impregnated in graphene oxide solution and carries out post-processing to get melamine is arrived Sponge-graphene oxide adsorbent material.
5. by the preparation method of melamine sponge-graphene oxide adsorbent material as claimed in claim 4, which is characterized in that It is slowly added to control its temperature in step 2 during potassium permanganate at 35 DEG C ~ 40 DEG C.
6. by the preparation method of melamine sponge-graphene oxide adsorbent material described in claim 4 or 5, feature exists In, centrifuge washing described in step 5) include using reagent 5% hydrochloric acid solution.
7. by the preparation method of melamine sponge-graphene oxide adsorbent material as claimed in claim 4, which is characterized in that Pretreatment described in step 6) is 80 DEG C of drying after cleaning melamine sponge with ethyl alcohol.
8. the sponge of the melamine as described in claim 4 or 5 or 7-graphene oxide adsorbent material preparation method, feature It is, post-processing described in step 6) is drying after melamine sponge is filled graphene oxide solution, then sponge is placed in In deionized water, carrying out washing treatment is carried out, is dried again later to get melamine sponge-graphene oxide adsorbent material.
CN201910277857.0A 2019-04-08 2019-04-08 A kind of melamine sponge-graphene oxide adsorbent material and its preparation method and application Pending CN110124629A (en)

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CN114195214A (en) * 2021-12-02 2022-03-18 中北大学 Method for constructing solar evaporator by using graphene oxide
CN115193409A (en) * 2022-07-15 2022-10-18 中国石油大学(华东) Photo-thermal adsorption heavy oil material based on modified melamine sponge, and preparation and application thereof

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CN108212083A (en) * 2017-12-28 2018-06-29 西南石油大学 A kind of oil suction carbon sponge and preparation method thereof

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Title
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刘韬: "氧化石墨烯复合材料的制备及在染料吸附中的应用", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114195214A (en) * 2021-12-02 2022-03-18 中北大学 Method for constructing solar evaporator by using graphene oxide
CN114195214B (en) * 2021-12-02 2023-05-12 中北大学 Method for constructing solar evaporator by using graphene oxide
CN115193409A (en) * 2022-07-15 2022-10-18 中国石油大学(华东) Photo-thermal adsorption heavy oil material based on modified melamine sponge, and preparation and application thereof

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Application publication date: 20190816