CN106902742A - A kind of porous activated carbon supported magnesium oxide composite and its preparation method and application - Google Patents

A kind of porous activated carbon supported magnesium oxide composite and its preparation method and application Download PDF

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CN106902742A
CN106902742A CN201710283917.0A CN201710283917A CN106902742A CN 106902742 A CN106902742 A CN 106902742A CN 201710283917 A CN201710283917 A CN 201710283917A CN 106902742 A CN106902742 A CN 106902742A
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activated carbon
magnesium oxide
zif
oxide composite
porous activated
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CN106902742B (en
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李立清
周柯
高正才
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Central South University
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    • 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
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/04Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • 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
    • B01J20/06Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2253/00Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10Inorganic adsorbents
    • B01D2253/102Carbon
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2258/00Sources of waste gases
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2259/00Type of treatment
    • B01D2259/45Gas separation or purification devices adapted for specific applications
    • B01D2259/4508Gas separation or purification devices adapted for specific applications for cleaning air in buildings

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Abstract

The invention discloses a kind of porous activated carbon supported magnesium oxide composite and preparation method and application;Composite (MgO ZIF 8C) is uniformly filled in by nano-MgO particle in porous activated carbon hole and uniform deposition is constituted in porous active carbon surface, its preparation method is by the use of zeolitic imidazolate framework material (ZIFs) as carbon precursor material, adulterated in ZIFs magnesium elements simultaneously, then be carbonized by high-temperature calcination and to form MgO ZIF 8C materials;The advantages of MgO ZIF 8C materials of preparation not only inherit the high specific surface areas of ZIF 8 and pore volume high, and the load factor of its magnesia is high, and good dispersion, good stability is difficult for drop-off;It is applied to the absorption of volatility organic pollutant, adsorption effect is excellent, is particularly suitable for the absorption of acetone.

Description

A kind of porous activated carbon supported magnesium oxide composite and its preparation method and application
Technical field
The present invention relates to a kind of VOC sorbing materials, more particularly to a kind of porous activated carbon supported magnesium oxide composite and Its preparation method, further relates to application of the porous activated carbon supported magnesium oxide composite in volatile gas acetone is adsorbed, Belong to new material technology field.
Background technology
Volatile organic contaminant (VOC) is that have the chemical combination for polluting property during a class is prevalent in indoor and outdoor air Thing, and acetone is the wherein representative compound of ketone, can produce high risks to human body, such as to human central nervous system The generation suppression of system, anesthetic effect, can embody liver, kidney and film gland etc. and cause damage under high concentration environment to people for a long time.At present Governing measure for the acetone gas in control air has a lot, and absorption method is one kind side that wherein economical maturity is commonly used the most Method.
The huge specific surface area of activated carbon and pore volume ensure that its adsorption treatment ability, have been widely used for purification, The fields such as Environmental capacity, catalysis.In order to improve the performance of activated carbon, the selective power that raising is more directed to target contaminant has Necessity is modified using certain technology to it.Wherein loaded modified is metal ion or compound is attached to activated carbon table On face, then because metal ion or compound have stronger adhesion to adsorbate, therefore can effectively increase activated carbon To the absorption property of some organic matters.Traditional carrying method has impregnation-calcination method, baking mixed method, admixture activation method, chemistry Vapor deposition method, sol-gal process.However, at present these carrying method preparation process complexity, cost of material high, bad dispersibility, The shortcomings of load capacity is small, constrains the development and application of this new material.So developing, a kind of physical and chemical performance is excellent to answer Mould assembly activated carbon has important practical significance.
Chinese patent (CN10251445A) discloses a kind of porous carbon adsorbent and preparation method and application.It is specific public The active component of adsorbent is opened for agraphitic carbon and metal oxide, its preparation method is in nitric acid by natural macromolecular material Impregnated in saline solution, then dry, be carbonized, obtained final product;While the porous carbon adsorbent of preparation has good adsorbent effect, also Strengthen the adsorption effect to anionic inorganic pollutant.Chinese patent (CN 102908979A) discloses a kind of porous magnesia The preparation method of high-efficiency adsorbent is specifically disclosed by loading magnesium salts in the duct of porous material and surface, is obtained by calcining Porous magnesia high-efficiency adsorbent;Porous material is at least one in activated carbon, diatomite, silica gel, molecular sieve, prepared by it Porous magnesia specific surface area it is big, the high adsorption capacity of heavy metal ion, saturated extent of adsorption is big, should with good industry Use prospect.In addition, (" preparation of magnesia/absorbent charcoal composite material and its Study on adsorption properties ", Hou Shaoqin, Chinese Sea is big Learn, Master's thesis in 2009) it is open with magnesium salts and paper-making black liquid, magnesium salts and merchandise active carbon as raw material, through carbon dioxide Activation prepares magnesia/absorbent charcoal composite material.These methods are manufactured almost exclusively by infusion process load magnesium salts, then by pyrocarbon Change or roasting etc. be come magnesia/absorbent charcoal composite material for preparing, these metal oxides it is dispersed uneven, load is surely Qualitative difference, and it is mainly used for the ionic compound in absorption water.
The content of the invention
For the defect that the magnesium oxide modified activated carbon of existing metal is present, it is an object of the invention to be to provide a kind of Magnesium oxide dispersion is uniform, load capacity is high, good stability porous activated carbon supported magnesium oxide composite.
Another object of the present invention be provide it is a kind of it is simple to operate, low cost prepare the porous activated carbon bear The method for carrying magnesium oxide composite material.
It is to provide the porous activated carbon supported magnesium oxide composite in absorption VOC that third object of the present invention is Application in aspect, the sorbing material for being particularly well suited as selective absorption acetone is used.
In order to realize above-mentioned technical purpose, the invention provides a kind of porous activated carbon supported magnesium oxide composite (MgO-ZIF-8C) preparation method, the method is that after zinc nitrate, magnesium salts and 2-methylimidazole are dissolved in into methyl alcohol respectively, ultrasound is mixed Close, ammoniacal liquor is added in gained mixed solution, stirring reaction separates out precipitated product;The precipitated product is by drying, carbonization, Obtain final product.
Technical scheme it is critical only that magnesium salts and the raw material one for preparing zeolitic imidazolate framework material (ZIFs) Rise and prepare carbon precursor material (ZIF-8), the ZIF-8 of preparation has specific surface area and pore volume higher, and has thermally-stabilised well Property, and magnesia presoma (magnesium hydroxide) uniform adsorption is supported in the cavity of ZIF-8 and skeleton surface, in carbonisation In, while the in-situ preparation of magnesium oxide nanoparticle is realized, so that magnesia is dispersed in porous carbon material, and oxygen Change magnesium in-situ preparation, its load stability is good.Compared with conventional carbon load technology, conventional carbon load oxidation is solved Magnesium exist load factor is low, poor dispersion, the technical barrier such as easy to fall off.
Preferred scheme, the mol ratio of zinc nitrate, magnesium salts and 2-methylimidazole is 1:0.5~5:0.5~5.By this hair Bright technical scheme prepares porous activated carbon supported magnesium oxide composite, and the concentration of magnesium salts can be in larger concentration range Regulated and controled, the porous activated carbon supported magnesium oxide composite that MgO-Supported amount is up to 30% can be obtained.
More preferably scheme, the magnesium salts is magnesium nitrate.
Preferred scheme, ammoniacal liquor is 2~3 with the volume ratio of methyl alcohol in mixed solution:1.
Preferred scheme, the temperature of stirring reaction is 10~40 DEG C, and the time is 3~8 hours.Technical scheme is led to Ultrasonic wave added dissolving is crossed, is conducive to solute to be preferably scattered in organic solvent, then by appropriate reaction temperature and time, have Beneficial to being formed, particle is smaller and particle uniform alumina magnesium.Can be by nano magnesia grain size Control at 2~10 nanometers In the range of.
Preferred scheme, the carbonisation:It is protection gas to employ nitrogen as, and is heated up with 5~10 DEG C/min heating rates To after 700~950 DEG C, make temperature stabilization at 700~950 DEG C, be incubated 1~3 hour.By selecting suitable heating rate, guarantor Temperature, soaking time, rate of temperature fall are conducive to ZIF-8C activated carbons to form bigger specific surface area and aperture.
More preferably scheme, zinc nitrate hexahydrate is dissolved in methyl alcohol and obtains the solution that concentration is 0.25~0.35mol/L.2- first Base imidazoles obtains the solution that concentration is 0.5~0.7mol/L after being dissolved in methyl alcohol.Preferred concentration range, advantageously forms structure steady Fixed complex.
Preferred scheme, with nitrogen as protective gas in carbonisation, is conducive to the abundant ZIF-8C porous knots of activated carbon Structure.
Present invention also offers a kind of porous activated carbon supported magnesium oxide composite, obtained by above-mentioned preparation method.
Preferred scheme, porous activated carbon supported magnesium oxide composite is uniformly filled in porous work by nano-MgO particle Property charcoal hole in and uniform deposition porous active carbon surface constitute.
Preferred scheme, nano magnesia grain size is 2~10 nanometers.Magnesia from appropriate particle diameter is brilliant Body, enables magnesia to be preferably embedded in the hole system of ZIF-8C activated carbons, enhances adhesion between the two.
More preferably scheme, the nano-MgO granular mass is the 1.0~30.0% of porous activated carbon quality.From appropriate Load capacity can either ensure that the dispersion of the nano magnesia for having enough is carried on ZIF-8C activated carbons, can simultaneously retain many again The larger specific surface area of hole Carbon Materials and aperture.
Present invention also offers the application of porous activated carbon supported magnesium oxide composite, it is applied to absorption volatile Property organic matter.
Preferred scheme, porous activated carbon supported magnesium oxide composite is used to adsorb third as absorption column material Ketone.Porous activated carbon supported magnesium oxide composite has stronger suction-operated to acetone, and one side activated carbon possesses big ratio Surface area and suitable aperture contribute to acetone gas in the absorption on its surface, on the other hand, are scattered in the magnesia in activated carbon There is the chemical actions such as the fracture of chemical bond and restructuring in meeting and acetone, can also promote absorption of the activated carbon to acetone.Both collaborations Effect, greatly improves suction-operated of the composite to acetone.
The method that the present invention prepares MgO-ZIF-8C includes step in detail below:
(1) by Zn (NO3)2·6H2O, 2-methylimidazole, Mg (NO3)2·6H2O is dissolved in methyl alcohol respectively, then by certain ratio Example ultrasonic mixing, during ammoniacal liquor added into mixed solution, in 10~40 DEG C of stirring reactions 3~8 hours, after the completion of reaction, filtering point From rear, H is used2O/MeOH(1:1V/V) methyl alcohol mixed solution is washed three times;
(2) gained solid will be separated by filtration after 90~100 DEG C of dryings 8~12 hours, will be placed in tube furnace, protected in nitrogen Under the conditions of shield, in calcining charing is carried out under 700~950 DEG C of temperature conditionss, MgO-ZIF-8C is obtained final product.
Compared with the prior art, the Advantageous Effects that technical scheme is brought:
1st, porous activated carbon supported magnesium oxide composite biggest advantage prepared by technical scheme is oxygen Change magnesium-supported amount big, and can be in interior regulation and control in a big way;Magnesium oxide dispersion is good, is uniformly filled in porous activated carbon hole And uniform deposition is in porous active carbon surface;Magnesia by in-situ deposition in porous carbon surface and hole, load stabilization, no Easy to fall off, solving active carbon supported magnesium oxide in the prior art, to there is load capacity small, and dispersion is uneven, and load stability is poor, Easy to fall off the problems such as.
2nd, the method for porous activated carbon supported magnesium oxide composite prepared by technical scheme is simple to operate, into This is low, meets demand of industrial production.
3rd, porous activated carbon supported magnesium oxide composite MgO-ZIF-8C can have obtained in technical scheme VOC in the absorption air of effect, particularly can be with selective absorption acetone gas;The bigger serface of one side activated carbon and hole Footpath contributes to acetone gas in the absorption on its surface, and on the other hand, the magnesia being scattered in activated carbon can also occur with acetone The chemical actions such as the fracture and restructuring of chemical bond, can also promote absorption of the activated carbon to acetone;Adsorption effect is obvious.
4th, technical scheme is by ZIFs as the template (presoma) for preparing porous carbon materials, and its materialization is stable Property it is good, with high-ratio surface and pore volume, the porous carbon aperture of preparation is relatively simple, and micropore is more and functional group abundant, compared to It is the ZIFs materials before carbonization, adsorption capacity is obviously improved.
Brief description of the drawings
【Fig. 1】A () is the XRD that embodiment 1 prepares MgO-ZIF-8C;B () is the XRD that embodiment 2 prepares ZIF-8C; C () is the XRD that embodiment 3 prepares MgO-AC.
【Fig. 2】A () is that MgO-ZIF-8C prepared by embodiment 1 is implementation to adsorption isothermal curve figure (b) of acetone gas The adsorption isothermal curve figure of MgO-ZIF-8C prepared by example 1 to toluene gas;C () is prepared by embodiment 1 MgO-ZIF-8C pairs The adsorption isothermal curve figure of benzene gas.
【Fig. 3】A () is the adsorption isothermal curve figures of the MgO-ZIF-8C to acetone gas of the preparation of embodiment 1;B () is implementation The adsorption isothermal curve figure of ZIF-8C prepared by example 2 to acetone gas;C () is the MgO-AC of the preparation of embodiment 3 to acetone gas Adsorption isothermal curve figure;D () is the adsorption isothermal curve figure of MgO-ZIF-8C prepared by embodiment 4.
Specific embodiment
Following examples are intended to further illustrate present invention, rather than the protection model of limitation the claims in the present invention Enclose.
Embodiment 1
By 7.2g Zn (NO3)2·6H2O, 4g 2-methylimidazole add conical flask in, be added thereto to 48mL without water beetle Alcoholic solution, ultrasonic wave dissolves 10 minutes.By 3.6g Mg (NO3)2·6H2O is added in conical flask, then be added thereto to 24mL without Water beetle alcoholic solution, then ultrasonic wave dissolving 10 minutes.Then by Zn (NO3)2·6H2O, 2-methylimidazole and Mg (NO3)2·6H2O Both solution mixing, add 180mL ammoniacal liquor afterwards, and 5 hours of magnetic stirrer are used under 20 DEG C, condition of normal pressure.
After reaction terminates, vavuum pump suction filtration is used, the solid product of collection is through H2O/MeOH(1:1V/V) methyl alcohol mixed solution Washing three times, finally 100 DEG C of dryings 12 hours in drying box, obtain the ZIF-8 materials containing Mg elements, are denoted as Mg-ZIF-8.
Mg-ZIF-8 materials will be prepared to be carbonized with tube furnace, the protective gas used during carbonization is nitrogen.By drying Mg-ZIF-8 after degasification is put into quartz boat, and quartz boat is put into tube furnace, and tube furnace uses temperature automatically controlled pattern, experiment During tube furnace reach 900 DEG C with the heating rate of 5 DEG C/min, be incubated 2 hours at 900 DEG C, during cooling first with 10 DEG C/ Min cools to 600 DEG C, then Temperature fall, is taken out after dropping to room temperature, the material for obtaining referred to as MgO-ZIF-8C.
Absorption property is tested:The compound activated carbon MgO-ZIF-8C that will be prepared is put into adsorption column, is adsorbed during experiment Post is incubated by 25 DEG C of waters bath with thermostatic control, with the gas flow of 50mL/min to being passed through certain density acetone gas in adsorption column Body, adsorption column exit concentration is measured by gas-chromatography.
The absorption test of different acetone concentrations:Every time N is first used before different acetone concentration tests are carried out2Gas is purged, Test experiments are carried out with the acetone gas of steady concentration again, test result is:
It is 40g/m in acetone gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 109mg/g.
It is 50g/m in acetone gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 188mg/g.
It is 60g/m in acetone gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 231mg/g.
It is 70g/m in acetone gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 256mg/g.
It is 80g/m in acetone gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 272mg/g.
The absorption test of different toluene concentrations:Every time N is first used before different toluene concentration tests are carried out2Gas is purged, Test experiments are carried out with the toluene gas of steady concentration again, test result is:
It is 40g/m in toluene gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 36mg/g.
It is 50g/m in toluene gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 39mg/g.
It is 60g/m in toluene gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 40mg/g.
It is 70g/m in toluene gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 43mg/g.
It is 80g/m in toluene gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 46mg/g.
The absorption test of different benzene concentrations:Every time N is first used before different benzene concentration tests are carried out2Gas is purged, then is used The benzene gas of steady concentration carry out test experiments, and test result is:
It is 40g/m in benzene gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 28mg/g.
It is 50g/m in benzene gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 31mg/g.
It is 60g/m in benzene gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 32mg/g.
It is 70g/m in benzene gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 34mg/g.
It is 80g/m in benzene gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 35mg/g.
One is respectively provided with to VOCs such as benzene, acetone and toluene by can be seen that MgO-ZIF-8C in embodiment 1 Fixed adsorption effect, but adsorption effect to acetone is significantly larger than other VOCs.
Embodiment 2
By 7.2g Zn (NO3)2·6H2O and 4g 2-methylimidazoles are separately added into two conical flasks, then are separately added into 36mL absolute methanol solutions, are dissolved 10 minutes with ultrasonic wave, it is fully dissolved, and then mix the two, and 180mL ammonia is added afterwards Water, uses 5 hours of magnetic stirrer under 20 DEG C, condition of normal pressure.After reaction terminates, use vavuum pump suction filtration, collection is consolidated Body product is through H2O/MeOH(1:1V/V) methyl alcohol mixed solution is washed three times, and finally 100 DEG C of dryings 12 hours in drying box, obtain To synthetic material, ZIF-8 is denoted as.ZIF-8 materials will be prepared to be carbonized with tube furnace, the protective gas used during carbonization is nitrogen Gas.The ZIF-8 after degasification will be dried to be put into quartz boat, quartz boat is put into tube furnace, tube furnace uses temperature automatically controlled mould Formula, tube furnace reaches 900 DEG C with the heating rate of 5 DEG C/min in experimentation, and 2 hours are incubated at 900 DEG C, during cooling first with 10 DEG C/min cools to 600 DEG C, then Temperature fall, is taken out after dropping to room temperature, the material for obtaining referred to as ZIF-8C.
Absorption property is tested:The compound activated carbon ZIF-8C that will be prepared is put into homemade adsorption column, is inhaled during experiment Attached column is incubated by 25 DEG C of waters bath with thermostatic control, with the gas flow of 50mL/min to being passed through certain density acetone gas in adsorption column Body, adsorption column exit concentration is measured by gas-chromatography.
The absorption test of different acetone concentrations:Every time N is first used before different acetone concentration tests are carried out2Gas is purged, Test experiments are carried out with the acetone gas of steady concentration again, test result is:
It is 40g/m in acetone gas concentration3When, activated carbon ZIF-8C adsorbances are 46mg/g.
It is 50g/m in acetone gas concentration3When, activated carbon ZIF-8C adsorbances are 87mg/g.
It is 60g/m in acetone gas concentration3When, activated carbon ZIF-8C adsorbances are 109mg/g.
It is 70g/m in acetone gas concentration3When, activated carbon ZIF-8C adsorbances are 122mg/g.
It is 80g/m in acetone gas concentration3When, activated carbon ZIF-8C adsorbances are 130mg/g.
As can be seen that for relative embodiment 1, when without doping magnesia, directly being carbonized by ZIF-8 in by implementing 2 To acetone with certain adsorption effect, but adsorption effect is much worse than the porous active of doping magnesia to the ZIF-8C for obtaining Carbon Materials MgO-ZIF-8C.Porous activated carbon is embodied well with the synergy of magnesia absorption acetone.
Embodiment 3
By 3.6g Mg (NO3)2·6H2O is added in conical flask, is added thereto to the distilled water of 100mL, ultrasonic wave dissolving 10 minutes.Treat Mg (NO3)2·6H2After O is completely dissolved, to addition 10.0g commercial activated carbons (Henan Changge) in the solution.Mixing Thing uses 5 hours of magnetic stirrer under 20 DEG C, condition of normal pressure.Then, with 80 DEG C of dryings in drying box, until evaporation Solvent is removed, the solid of gained continues to be dried 12 hours at 100 DEG C, obtains activated carbon (AC) material containing Mg elements, is denoted as Mg-AC。
Mg-AC materials will be prepared to be carbonized with tube furnace, the protective gas used during carbonization is nitrogen.Degasification will be dried Mg-ZIF-8 afterwards is put into quartz boat, and quartz boat is put into tube furnace, and tube furnace uses temperature automatically controlled pattern, experimentation Middle tube furnace reaches 550 DEG C with the heating rate of 5 DEG C/min, and 2 hours are incubated at 550 DEG C, and then Temperature fall, drops to room temperature After take out, the material for obtaining referred to as MgO-AC.
Absorption property is tested:The compound activated carbon ZIF-8C that will be prepared is put into homemade adsorption column, is inhaled during experiment Attached column is incubated by 25 DEG C of waters bath with thermostatic control, with the gas flow of 50mL/min to being passed through certain density acetone gas in adsorption column Body, adsorption column exit concentration is measured by gas-chromatography.
The absorption test of different acetone concentrations:Every time N is first used before different acetone concentration tests are carried out2Gas is purged, Test experiments are carried out with the acetone gas of steady concentration again, test result is:
It is 40g/m in acetone gas concentration3When, compound activated carbon MgO-AC adsorbances are 79mg/g.
It is 50g/m in acetone gas concentration3When, compound activated carbon MgO-AC adsorbances are 141mg/g.
It is 60g/m in acetone gas concentration3When, compound activated carbon MgO-AC adsorbances are 173mg/g.
It is 70g/m in acetone gas concentration3When, compound activated carbon MgO-AC adsorbances are 188mg/g.
It is 80g/m in acetone gas concentration3When, compound activated carbon MgO-AC adsorbances are 201mg/g.
As can be seen that for relative embodiment 1, directly loading oxygen by infusion process using commercial activated carbons in by implementing 3 Change magnesium, to acetone with preferable adsorption effect, but adsorption effect is porous much worse than doping magnesia for the MgO-AC for obtaining Absorbent charcoal material MgO-ZIF-8C.Mainly infusion process prepare MgO-AC load capacity is relatively low, stability is poor, and business is living Property the ZIF-8C pore structures that prepare of charcoal and ZIF-8 charing it is relatively poor.
Embodiment 4
By 7.2g Zn (NO3)2·6H2O, 4g 2-methylimidazole add conical flask in, be added thereto to 48mL without water beetle Alcoholic solution, ultrasonic wave dissolves 10 minutes.By 2.5g Mg (NO3)2·6H2O is added in conical flask, then be added thereto to 24mL without Water beetle alcoholic solution, then ultrasonic wave dissolving 10 minutes.Then by Zn (NO3)2·6H2O, 2-methylimidazole and Mg (NO3)2·6H2O Both solution mixing, add 180mL ammoniacal liquor afterwards, and 5 hours of magnetic stirrer are used under 20 DEG C, condition of normal pressure.
After reaction terminates, vavuum pump suction filtration is used, the solid product of collection is through H2O/MeOH(1:1V/V) methyl alcohol mixed solution Washing three times, finally 100 DEG C of dryings 12 hours in drying box, obtain the ZIF-8 materials containing Mg elements, are denoted as Mg-ZIF-8.
Mg-ZIF-8 materials will be prepared to be carbonized with tube furnace, the protective gas used during carbonization is nitrogen.By drying Mg-ZIF-8 after degasification is put into quartz boat, and quartz boat is put into tube furnace, and tube furnace uses temperature automatically controlled pattern, experiment During tube furnace reach 800 DEG C with the heating rate of 5 DEG C/min, be incubated 2 hours at 800 DEG C, during cooling first with 10 DEG C/ Min cools to 600 DEG C, then Temperature fall, is taken out after dropping to room temperature, the material for obtaining referred to as MgO-ZIF-8C.
Absorption property is tested:The compound activated carbon MgO-ZIF-8C that will be prepared is put into adsorption column, is adsorbed during experiment Post is incubated by 25 DEG C of waters bath with thermostatic control, with the gas flow of 50mL/min to being passed through certain density acetone gas in adsorption column Body, adsorption column exit concentration is measured by gas-chromatography.
The absorption test of different acetone concentrations:Every time N is first used before different acetone concentration tests are carried out2Gas is purged, Test experiments are carried out with the acetone gas of steady concentration again, test result is:
It is 40g/m in acetone gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 86mg/g.
It is 50g/m in acetone gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 159mg/g.
It is 60g/m in acetone gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 189mg/g.
It is 70g/m in acetone gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 206mg/g.
It is 80g/m in acetone gas concentration3When, compound activated carbon MgO-ZIF-8C adsorbances are 221mg/g.

Claims (10)

1. a kind of preparation method of porous activated carbon supported magnesium oxide composite, it is characterised in that:By zinc nitrate, magnesium salts and 2- After methylimidazole is dissolved in methyl alcohol respectively, ultrasonic mixing adds ammoniacal liquor in gained mixed solution, and stirring reaction separates out precipitation and produces Thing;The precipitated product is by drying, carbonization, obtains final product.
2. the preparation method of porous activated carbon supported magnesium oxide composite according to claim 1, it is characterised in that:Nitre The mol ratio of sour zinc, magnesium salts and 2-methylimidazole is 1:0.5~5:0.5~5;The magnesium salts is magnesium nitrate.
3. the preparation method of porous activated carbon supported magnesium oxide composite according to claim 1, it is characterised in that:Ammonia Water is 2~3 with the volume ratio of methyl alcohol in mixed solution:1.
4. the preparation method of the porous activated carbon supported magnesium oxide composite according to any one of claims 1 to 3, it is special Levy and be:The temperature of stirring reaction is 10~40 DEG C, and the time is 3~8 hours.
5. the preparation method of the porous activated carbon supported magnesium oxide composite according to any one of claims 1 to 3, it is special Levy and be:The carbonisation:It is protection gas to employ nitrogen as, and 850~950 DEG C are warming up to 5~10 DEG C/min heating rates Afterwards, make temperature stabilization at 700~950 DEG C, be incubated 1~3 hour.
6. a kind of porous activated carbon supported magnesium oxide composite, it is characterised in that:As described in any one of claim 1~6 Preparation method is obtained.
7. porous activated carbon supported magnesium oxide composite according to claim 6, it is characterised in that:By nano-MgO Grain is uniformly filled in porous activated carbon hole and uniform deposition is constituted in porous active carbon surface.
8. porous activated carbon supported magnesium oxide composite according to claim 7, it is characterised in that:The nano-MgO Granular mass is the 1.0~30.0% of porous activated carbon quality;The nano-MgO grain size is 2~10 nanometers.
9. the application of the porous activated carbon supported magnesium oxide composite described in any one of claim 6~8, it is characterised in that: It is applied to adsorb VOC.
10. the application of porous activated carbon supported magnesium oxide composite according to claim 9, it is characterised in that:As Absorption column material is used to adsorb acetone.
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CN110652961A (en) * 2019-10-08 2020-01-07 安徽建筑大学 Preparation method of magnesium oxide porous nano material loaded activated carbon fiber felt
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