CN108393067A - A kind of method, its product and the application of fabricated in situ mangano-manganic oxide/graphene composite adsorbent - Google Patents

A kind of method, its product and the application of fabricated in situ mangano-manganic oxide/graphene composite adsorbent Download PDF

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CN108393067A
CN108393067A CN201810286119.8A CN201810286119A CN108393067A CN 108393067 A CN108393067 A CN 108393067A CN 201810286119 A CN201810286119 A CN 201810286119A CN 108393067 A CN108393067 A CN 108393067A
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graphene
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CN108393067B (en
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李英儒
任鸣
任一鸣
邵浪
唐浩
蔡定洲
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • B01J20/205Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/288Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • GPHYSICS
    • G21NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21FPROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/04Treating liquids
    • G21F9/06Processing
    • G21F9/12Processing by absorption; by adsorption; by ion-exchange
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/006Radioactive compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/08Seawater, e.g. for desalination

Abstract

The invention discloses a kind of method, its product and the applications of fabricated in situ mangano-manganic oxide/graphene composite adsorbent, belong to uranyl ion sorbing material preparation field, its object is to solve the problems, such as the separation, recycling of uranium in water body.The present invention is based on modified Hummers methods, propose a kind of preparation method of fabricated in situ mangano-manganic oxide/graphene composite adsorbent, and are related to it and inhale appended application in uranyl.The application is based on being improved traditional Hummers methods, it is proposed that the method that nano manganic manganous oxide/redox graphene compound adsorbent is prepared in situ in a step.The compound adsorbent that this method is prepared has higher equilibrium adsorption capacity for uranyl ion, and avoids complicated cumbersome post-processing purification process.Meanwhile the present invention can make full use of the manganese element of potassium permanganate in raw material, reduce the discharge of heavy metal wastewater thereby.In addition, the waste water generated is alkalescent, facilitate the post-processing of waste liquid.The present invention has the characteristics that production cost is low, is easily enlarged production.

Description

A kind of method of fabricated in situ mangano-manganic oxide/graphene composite adsorbent, its product And application
Technical field
The present invention relates to sorbing material preparation fields, especially uranyl ion sorbing material preparation field, specially a kind of Method, its product and the application of fabricated in situ mangano-manganic oxide/graphene composite adsorbent.
Background technology
Environment and the energy are the bases that the mankind depend on for existence and development, with the development of science and technology, nuclear energy the mankind production, More and more important role is played in life.The year two thousand twenty is expected, the installed capacity of China's nuclear power accounts for the proportion of gross generation It will be promoted to 7 % or so from 2 current %.Supply capacity and spentnuclear fuel of the rapid development of China's nuclear undertaking to nuclear fuel Processing capacity all bring stern challenge.
Uranium be both nuclear fuel main component and spentnuclear fuel last handling process in need one of main nucleic to be separated. In the exploitation, ore dressing, smelting of uranium ore, the preparation of nuclear fuel, processing, separation of spentnuclear fuel etc. relate in uranium operation, are likely to produce The waste water of raw uranium-bearing.And uranium having chemical toxicity and radioactive heavy metal as a kind of, if be discharged into natural environment, It accumulates in the natural environment, it is possible to cause the background radiation of environment to increase, and then cause the gene of wild animal and plant prominent Become, potential threaten is constituted to the survival and development of the mankind.Therefore, dealing carefully with for uranium-containing waste water, has great importance.
On the other hand, with the development of nuclear power, nuclear industry is growing day by day for the demand of uranium.However, the storage of land uranium ore It measures limited.The concentration of URANIUM IN SEAWATER is relatively low, but the total amount of seawater is very huge, this makes the total amount of URANIUM IN SEAWATER considerably beyond land The uranium content of ground uranium ore.Therefore, the extraction of uranium from seawater is likely to be the main path that the following mankind obtain uranium resource.
In conclusion being detached in water body, recycling uranium with important scientific meaning and application value.Absorption method has behaviour Make simple, favorable repeatability, be easily enlarged production, it is applied widely the advantages that, be expected to solve uranium separation in water body, recycle Problem, and adsorbent is then its key factor.Therefore, developing cheap, efficient uranium absorption agent has important scientific meaning, It is the field one of significant problem urgently to be resolved hurrily.
Invention content
The goal of the invention of the present invention is:Separation, recycling for uranium in water body provide a kind of cheap, efficient uranium suction It attached dose, is more specifically to provide a kind of method of fabricated in situ mangano-manganic oxide/graphene composite adsorbent, its product and answers With.The present invention is based on modified Hummers methods, propose a kind of preparation of fabricated in situ mangano-manganic oxide/graphene composite adsorbent Method, and be related to it and inhale appended application in uranyl.The application is based on being improved traditional Hummers methods, it is proposed that a step The method that nano manganic manganous oxide/redox graphene compound adsorbent is prepared in situ.The composite adsorption that this method is prepared Agent has higher equilibrium adsorption capacity for uranyl ion, and avoids complicated cumbersome post-processing purification process.Meanwhile this hair It is bright the manganese element of potassium permanganate in raw material to be made full use of, reduce the discharge of heavy metal wastewater thereby.In addition, the waste water generated is weak Alkalinity facilitates the post-processing of waste liquid.The present invention has the characteristics that production cost is low, is easily enlarged production.
To achieve the goals above, the present invention adopts the following technical scheme that:
A kind of method of fabricated in situ mangano-manganic oxide/graphene composite adsorbent, includes the following steps:
(1)Graphite powder, the concentrated sulfuric acid and potassium permanganate are mixed and carry out oxidation reaction, obtains graphite oxide pulpous state product;To gained Deionized water is added in graphite oxide pulpous state product and hydrogen peroxide obtains graphene oxide to restore unreacted potassium permanganate Suspension;
(2)Gained graphene oxide suspension is adjusted into pH value to alkalinity, obtains the second reaction product;
(3)Second reaction product is evaporated, third solid product is obtained, third solid product is heat-treated, with To crude product;
(4)With deionized water to step(3)Gained crude product carries out washing impurity-removing, and drying obtains mangano-manganic oxide/graphene essence Product, you can;
The step(1)In, the mass ratio of graphite powder, the concentrated sulfuric acid and potassium permanganate is 1:30-70:(4-5).
In the step 1, oxidizing reaction temperature is 30 ~ 50 DEG C, and the reaction time is 0.5 ~ 2h.
In the step 1, under the conditions of ice-water bath and magnetic agitation, the concentrated sulfuric acid is first added into reaction kettle, waits for reaction kettle When interior concentrated sulfuric acid temperature is reduced to 5 DEG C or less, then potassium permanganate is added thereto, and temperature of reaction system is made to be maintained at 5 DEG C Hereinafter, after stirring evenly, then graphite powder is added thereto, obtain the first mixed reactant;First mixed reactant is warming up to 30 ~ 50 DEG C, 0.5 ~ 2h is reacted, until the first mixed reactant is transformed into dark thick slurry, i.e. pulpous state product;First starched to gained Deionized water is added in shape product, then hydrogen peroxide is added thereto, to restore unreacted potassium permanganate, until reaction suspension turns Become glassy yellow, i.e. graphene oxide suspension.
In the step 2, alkaline matter is added into the suspended liquor of step 1 gained graphene oxide, adjusts graphite oxide Alkene suspension pH value is supported on so as to which mangano-manganic oxide is obtained by the reaction on graphene oxide to alkalinity.
Into the suspended liquor of step 1 gained graphene oxide plus the alkaline matter of molar excess, the alkaline matter are It is one or more in potassium hydroxide, sodium hydroxide.
In terms of the concentrated sulfuric acid, the molar ratio of alkaline matter and the concentrated sulfuric acid is (19 ~ 24):9;Preferably, molar ratio is 20:9.
In the step 3, evaporation operation is as follows:Second reaction product is boiled, the temperature of evaporation is 120 ~ 150 DEG C.
In the step 3, evaporation gained third solid product is handled into 3 ~ 10h at 160 ~ 250 DEG C, is realized solid to third The thermal reduction of body product, to obtain crude product;Preferably, evaporation gained third solid product is handled 3 at 170 ~ 200 DEG C ~5h。
It further include last handling process:Step 4 gained mangano-manganic oxide/graphene essence product is subjected to ball-milling treatment, is obtained Mangano-manganic oxide/graphene powder.
Ball-milling treatment condition is as follows:300 ~ 500r/min of rotating speed, time are 4 ~ 8h.
Using the product prepared by preceding method.
Using application of the mangano-manganic oxide/graphene composite adsorbent prepared by preceding method in uranyl processing.
By the adsorbent in uranium-containing waste water processing, the processing of natural stream networks uranium or the extraction of uranium from seawater.
Mangano-manganic oxide is a kind of black or the crystal of brown, belongs to tetragonal crystal system spinel structure.Ionic structure is Mn2+ (Mn3+)2O4, oxygen atom is cubic close accumulation, and Mn2+ occupies tetrahedron gap, and Mn3+ occupies octahedral interstices.In nature Exist in the form of hausmannite, is most stable of oxide.Wherein, mangano-manganic oxide surface has abundant hydroxyl, for very much Heavy metal species and organic compound have strong absorption and enrichment, and in existing research work, mangano-manganic oxide is aobvious It shows for the strong suction-operated of the heavy metal ion such as cadmium, chromium, lead, zinc.
Graphene as a kind of novel two-dimension nano materials, with excellent mechanical performance, huge specific surface area, Thermal conductivity, good chemical stability, thermal stability.In addition, as a kind of carbon material, the radiation resistance of graphene It can be also more outstanding.Therefore, since being found, graphene has shown certain application potential in numerous areas, as can Measure conversion, energy stores, Material reinforcement, lubrication, absorption etc..Currently, being most to have on a large scale using the method for chemistry redox The method for preparing grapheme material of industrialization potential.Wherein, in concentrated sulfuric acid medium, potassium permanganate oxidation graphite is utilized Hummers methods are widely used.But this method, which there are still some drawbacks, to be needed to solve, such as:1)Generation largely contains heavy metal The strongly acid wastewater of manganese ion, 2)There is still a need for the purification steps of further complexity for the graphene oxide of preparation.
For foregoing problems, think after applicant's research, a kind of excellent adsorbent should have and can have with adsorbate Compared with the functional group of strong interaction, there is higher specific surface area again, and then can fully have an effect with adsorbate.And four There is unpaired electron in Mn 3 O structure, there is certain magnetism, can divide from aqueous systems under the action of high-intensity magnetic field From.And the size of nano particle in 100 nm hereinafter, have very high specific surface area.Therefore, applicant thinks Mn oxide The compound of nano-particle and graphene is expected to become a kind of excellent adsorbent.Further, mangano-manganic oxide is processed into and is received Rice material, and appropriate means is taken to prevent its aggregation, it can further promote its adsorption effect.
For this purpose, the present invention provide a kind of method of fabricated in situ mangano-manganic oxide/graphene composite adsorbent, its product and Using being a kind of simple and efficient method for preparing mangano-manganic oxide/redox graphene compound adsorbent.When it is prepared, Graphite powder is mixed with potassium permanganate to and carried out oxidation reaction in concentrated sulfuric acid first, obtains graphite oxide pulpous state product;To oxygen Deionized water and hydrogen peroxide are sequentially added in graphite pulpous state product, to restore unreacted potassium permanganate, to be aoxidized Graphite suspension.The pH of gained graphene oxide suspension is adjusted to alkalinity, method is that the alkali of molar excess is added(I.e. by adding Adding the pH value of alkali solid or alkaline solution adjusting graphene oxide suspension, alkali solid can be hydroxide to alkalinity Potassium, sodium hydroxide, alkaline solution can be potassium hydroxide, sodium hydroxide solution), so that mangano-manganic oxide is obtained by the reaction and loads On the graphene oxide.Then, the mixture after adjusting pH value is evaporated, to obtain solid product, by solid Product carries out thermal reduction processing, to obtain mangano-manganic oxide/graphene crude product.Then, then by mangano-manganic oxide/graphene Removing impurity is washed with deionized in crude product, drying, to obtain mangano-manganic oxide/graphene essence product.Finally, by four oxygen Change three manganese/graphene essence product and carry out ball-milling treatment, uniform mangano-manganic oxide/graphene powder is refined to obtain size, That is mangano-manganic oxide/graphene composite adsorbent.In a specific example, ball milling, ball milling are carried out using high energy ball mill Tank volume is 50-100 ml, and ball milling ball is 3 mm and 1 mm mixed grinding balls, and single quality of the ball mill is 1-5 g, and rotational speed of ball-mill is 300 ~ 500 revs/min, Ball-milling Time is 4 ~ 8 hours.
To sum up, the present invention provides a kind of based on modified Hummers methods fabricated in situ mangano-manganic oxide/graphene composite adsorption The preparation method of agent, its application of the adsorbent and the adsorbent that prepare in uranyl ion etc. is heavy metal ion adsorbed.It is Graphite is used into potassium permanganate oxidation in sulfuric acid medium, deionized water dilution is added, it is straight to the graphite oxide dispersion after dilution Ground connection is slowly added to strong alkali solution or solid(Such as potassium hydroxide, sodium hydroxide etc.), make solution ph > 7, water will be dissolved in Manganese ion be converted to nano-particle precipitation.The sediment is heat-treated again, deionized water is used in combination repeatedly to rinse, is dried, Ball mill grinding obtains mangano-manganic oxide/graphene composite adsorbent.
After measured, adsorbent of the invention has higher equilibrium adsorption capacity for uranyl, and since mangano-manganic oxide has There is certain magnetism, can be removed adsorbent by high-intensity magnetic field, effectively simplifies last handling process.Meanwhile the present invention does not need pair Graphite oxide purify, and direct in-situ synthesizes compound adsorbent, and method is easy, cost relative reduction, have preferable Market application prospect.
Further, application of the adsorbent in uranyl processing is claimed in the present invention.Through practical measurement, the present invention containing The fields such as uranium wastewater treatment, the processing of natural stream networks uranium, the extraction of uranium from seawater have wide application potential.
Description of the drawings
Examples of the present invention will be described by way of reference to the accompanying drawings, wherein:
Fig. 1 is mangano-manganic oxide/graphene complex transmission electron microscope figure prepared by the present invention.
Fig. 2 is mangano-manganic oxide/graphene complex Raman curve graph prepared by the present invention.
Fig. 3 is mangano-manganic oxide/graphene complex XRD diagram prepared by the present invention.
Fig. 4 is equilibrium adsorption curve graph of the mangano-manganic oxide/graphene complex of the invention prepared to uranyl.
Specific implementation mode
All features disclosed in this specification or disclosed all methods or in the process the step of, in addition to mutually exclusive Feature and/or step other than, can combine in any way.
Any feature disclosed in this specification unless specifically stated can be equivalent or with similar purpose by other Alternative features are replaced.That is, unless specifically stated, each feature is an example in a series of equivalent or similar characteristics .
Embodiment 1
(1)Under conditions of ice-water bath, magnetic agitation, 75 ml are added into beaker(1.35 mol)The concentrated sulfuric acid waits for temperature reduction To 5 DEG C hereinafter, being slowly added to 10 g thereto again(0.065 mol)Potassium permanganate makes system temperature be no more than 5 DEG C;Stirring After uniformly, the graphite powder of 2.5 g, 600 mesh is added thereto;And reactant is warming up to 40 DEG C, 1.0h is kept, until reactant It is transformed into brownish black thick slurry.It is slowly added to 250 mL deionized waters into gained brownish black thick slurry, then adds Enter 30 % hydrogen peroxide reduction potassium permanganate, until gained suspension is transformed into glassy yellow to get to glassy yellow suspension.
(2)To step(1)The NaOH solution of 500 mL, 6 mol/L is slowly added in middle gained glassy yellow suspension(NaOH Total amount is 3 mol, 120 g), suspension is changed into alkaline black suspension.
(3)By step(2)Middle gained alkalinity black suspension is boiled, and is removed moisture, is obtained black third solid product.So Afterwards, gained third solid product is handled 4 h under conditions of 180 DEG C, obtains dark brown solid as in Muffle furnace(It is i.e. thick Product).
(4)By step(3)Gained dark brown solid(That is crude product)Again it is dispersed in water, filters, and wash repeatedly, remove Soluble saline and alkaline impurity is removed, then gained filter cake is placed in convection oven, is dried at 90 DEG C, obtains mangano-manganic oxide/stone Black alkene essence product.
(5)By step(4)Gained mangano-manganic oxide/graphene essence product carries out ball mill grinding processing, obtains uniform powder, That is mangano-manganic oxide/graphene composite adsorbent.Ball milling condition is as follows:Ball milling speed is 300 r/min, and processing time is 4 h; Abrading-ball is the agate abrading-ball of 3 mm and 1 mm, and two kinds of mill ball quality ratios are 1:1.
(6)Obtained mangano-manganic oxide/graphene nanometer composite is brownish-yellow powder.Transmission electron microscope(TEM) Display graphene is rendered as lamellar structure, and mangano-manganic oxide is rendered as irregular nano particle, is uniformly adhered to graphene Above lamella(Fig. 1).Raman presents two groups of strong peaks, and first group is 610 cm-1 That locates is unimodal, is the spy of mangano-manganic oxide Levy peak.Second group is 1350 cm-1、1560 cm-1Two strong peak and in 2700 ~ 3200 cm-1 Locate multiple short peaks, is oxygen reduction The characteristic peak of graphite alkene(Fig. 2).X-ray diffraction is the result shows that trimanganese tetroxide particle is spinel structure(Fig. 3).Absorption etc. Warm curve shows that the adsorbance of this compound adsorbent has reached 210 mg/g.
Embodiment 2
(1)Under conditions of ice-water bath, magnetic agitation, 75 mL are added in beaker(1.35 mol)The concentrated sulfuric acid waits for temperature reduction To 5 DEG C hereinafter, being slowly added to 10 g thereto again(0.065 mol)Potassium permanganate makes system temperature be no more than 5 DEG C;Stirring After uniformly, the graphite powder of 2.5 g, 600 mesh is added thereto;And reactant is warming up to 45 DEG C, 1.0h is kept, until reactant turns Become brownish black thick slurry.It is slowly added to 1000 mL deionized waters into gained brownish black thick slurry, then adds Enter 30 % hydrogen peroxide reduction potassium permanganate, until suspension is transformed into glassy yellow to get to glassy yellow suspension.
(2)To step(1)120 g NaOH solids are slowly added in middle gained glassy yellow suspension(NaOH total amounts are 3 mol), suspension is changed into alkaline black suspension.
(3)By step(2)Middle gained alkalinity black suspension is boiled, and is removed moisture, is obtained black third solid product.So Afterwards, gained third solid product is handled 4 h under conditions of 180 DEG C, obtains dark brown solid as in Muffle furnace(It is i.e. thick Product).
(4)By step(3)Gained dark brown solid(That is crude product)Again it is dispersed in water, filters, and wash repeatedly, remove Soluble saline and alkaline impurity is removed, then filtering gained filter cake is placed in convection oven, is dried at 90 DEG C, obtains four oxidations three Manganese/graphene essence product.
(5)By step(4)Middle gained mangano-manganic oxide/graphene essence product carries out ball mill grinding processing, obtains uniform powder End, i.e. mangano-manganic oxide/graphene composite adsorbent.Ball milling condition is as follows:Ball milling speed is 300 r/min, processing time 4 h;Abrading-ball is the agate abrading-ball of 3 mm and 1 mm, and two kinds of mill ball quality ratios are 1:1.
The invention is not limited in specific implementation modes above-mentioned.The present invention, which expands to, any in the present specification to be disclosed New feature or any new combination, and disclose any new method or process the step of or any new combination.

Claims (10)

1. a kind of method of fabricated in situ mangano-manganic oxide/graphene composite adsorbent, which is characterized in that include the following steps:
(1)Graphite powder, the concentrated sulfuric acid and potassium permanganate are mixed and carry out oxidation reaction, obtains graphite oxide pulpous state product;To gained Deionized water is added in graphite oxide pulpous state product and hydrogen peroxide obtains graphene oxide to restore unreacted potassium permanganate Suspension;
(2)Gained graphene oxide suspension is adjusted into pH value to alkalinity, obtains the second reaction product;
(3)Second reaction product is evaporated, third solid product is obtained, third solid product is heat-treated, with To crude product;
(4)With deionized water to step(3)Gained crude product carries out washing impurity-removing, and drying obtains mangano-manganic oxide/graphene essence Product, you can;
The step(1)In, the mass ratio of graphite powder, the concentrated sulfuric acid and potassium permanganate is 1:30-70:(4-5).
2. the method for fabricated in situ mangano-manganic oxide/graphene composite adsorbent according to claim 1, which is characterized in that In the step 1, oxidizing reaction temperature is 30 ~ 50 DEG C, and the reaction time is 0.5 ~ 2h.
3. the method for fabricated in situ mangano-manganic oxide/graphene composite adsorbent according to claim 2, which is characterized in that In the step 1, under the conditions of ice-water bath and magnetic agitation, the concentrated sulfuric acid is first added into reaction kettle, waits for the dense sulphur in reaction kettle When sour temperature is reduced to 5 DEG C or less, then potassium permanganate is added thereto, and temperature of reaction system is made to be maintained at 5 DEG C hereinafter, stirring After uniformly, then graphite powder is added thereto, obtains the first mixed reactant;First mixed reactant is warming up to 30 ~ 50 DEG C, instead 0.5 ~ 2h is answered, until the first mixed reactant is transformed into dark thick slurry, i.e. pulpous state product;First add into gained pulpous state product Enter deionized water, then hydrogen peroxide be added thereto, to restore unreacted potassium permanganate, until reaction suspension be transformed into it is bright orange Color, i.e. graphene oxide suspension.
4. the method for fabricated in situ mangano-manganic oxide/graphene composite adsorbent according to claim 1, which is characterized in that In the step 2, alkaline matter is added into the suspended liquor of step 1 gained graphene oxide, adjusts graphene oxide suspension PH value is supported on so as to which mangano-manganic oxide is obtained by the reaction on graphene oxide to alkalinity.
5. the method for fabricated in situ mangano-manganic oxide/graphene composite adsorbent according to claim 4, which is characterized in that Into the suspended liquor of step 1 gained graphene oxide plus molar excess alkaline matter, the alkaline matter be potassium hydroxide, It is one or more in sodium hydroxide.
6. special according to the method for any one of the claim 1 ~ 5 fabricated in situ mangano-manganic oxide/graphene composite adsorbent Sign is that in the step 3, evaporation operation is as follows:Second reaction product is boiled, the temperature of evaporation is 120 ~ 150 DEG C.
7. special according to the method for any one of the claim 1 ~ 6 fabricated in situ mangano-manganic oxide/graphene composite adsorbent Sign is, in the step 3, evaporation gained third solid product is handled 3 ~ 10h at 160 ~ 250 DEG C, is realized solid to third The thermal reduction of body product, to obtain crude product;Preferably, evaporation gained third solid product is handled 3 at 170 ~ 200 DEG C ~5h。
8. the product prepared using any one of preceding claims 1 ~ 7 the method.
9. mangano-manganic oxide/the graphene composite adsorbent prepared using any one of preceding claims 1 ~ 7 the method is in uranium Application in acyl processing.
10. application according to claim 9, which is characterized in that by the adsorbent for uranium-containing waste water processing, natural stream networks In uranium processing or the extraction of uranium from seawater.
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曹克诚等: "还原氧化石墨烯膜用于模拟核工业废水中铀酰离子的选择性筛分", 《中国知网》 *

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109879482A (en) * 2019-04-10 2019-06-14 华东交通大学 A kind of method of high magnetic graphene catalytic treatment coking wastewater
CN113089016A (en) * 2021-03-10 2021-07-09 西南科技大学 Preparation method of high-performance single-center uranium-based supported catalyst
CN113512449A (en) * 2021-07-09 2021-10-19 清华大学 Composite lubricating material and preparation method thereof

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