CN106629590A - Preparation method of novel ZIF-8 (Zeolitic Imidazolate Framework-8) clad n-octadecane phase-change gas-storage material - Google Patents
Preparation method of novel ZIF-8 (Zeolitic Imidazolate Framework-8) clad n-octadecane phase-change gas-storage material Download PDFInfo
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
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Abstract
The invention discloses a preparation method of a novel ZIF-8 (Zeolitic Imidazolate Framework-8) clad n-octadecane phase-change gas-storage material. The ZIF-8 clad n-octadecane phase-change gas-storage material is prepared by an emulsification method; sodium dodecyl sulfate (SDS, analytically pure) is first dissolved in deionized water; thawed n-octadecane (NOD) is added into an obtained first mixture for emulsification; afterwards, dimethyl imidazole is added into an obtained second mixture, so as to form an organometallic framework structure; thus, a structure-varied flower-similar type nano-structure phase-change gas-storage material is prepared through shaker cooling, suction filtration, the multiple washing with the deionized water, centrifugal separation and vacuum drying. Along with the change of a reaction condition, structures in various flower forms are formed. The structures have large specific surface areas; the phase-change temperature of the NOD is improved; the material has a hydrogen-storage function. ZIF-8 self is nontoxic; further, a reaction is carried out in a water environment; an organic solvent is not needed; the encapsulation rate is high; the stability is good; the preparation method is simple; the requirement on a device is low; the cost is low; the preparation method is environmentally-friendly.
Description
Technical field
The present invention relates to a kind of new ZIF-8 coats the preparation method of n-octadecane phase transformation gas storage material, more particularly to
A kind of method that nano material coats phase-change material, belongs to organometallic skeletal（MOFs）, nano material, the energy, gas storage
Field.
Background technology
As the mankind constantly rise to the demand of resource, coal, the mineral resources such as oil far can not meet people
Demand, and the high pollution that coal equal energy source has also makes people's headache the characteristics of consume big, reserves are low.Novel green can be again
The raw energy has allowed people to look forward to sth. with great eagerness.And Hydrogen Energy as the high green energy resource of a kind of rich reserves, wide material sources, energy density and
Energy carrier brings Gospel to human society.Hydrogen is present in a gaseous form at typical condition, and inflammable, explosive, easy diffusion,
Thus carry out very big inconvenience to storage and conveyer belt.The transport of safe efficient and No leakage loss is that today's society various countries generally close
The problem of note.Whole storage and transport process energy density (including quality hydrogen-storage density and volume hydrogen-storage density) height, energy are met simultaneously
The few requirement of consumption.There is the governed hydrogen storage method of mark there are following a few classes at present：High pressure compressed storage, liquid hydrogen storage, metal hydride
Storage, complex hydrides storage, porous adsorbent storage and chemical reaction storage.This several method is present in varying degrees
Shortcoming or limitation.The hydrogen storage process of such as high pressure compressed storage needs to consume extra work done during compression, and release hydrogen process needs extra
Stress control.And the material to high-pressure bottle itself also has very high requirement.Liquid hydrogen storage needs thick and heavy container, liquefaction
Process needs to consume substantial amounts of energy, and also evaporation loss.Metal hydride storage has hydrogen-storage density low and hydrogen discharging speed
Slow the problems such as.Zeolites porous mineral materials are due to itself having relatively large unit mass, while containing many in material
The major diameter space of hydrogen can not be inhaled, hydrogen storage effect is also not satisfactory.To sum up, above technology is all unsuitable for the big rule of hydrogen storage engineering
Mould is carried out, and phase transformation n-octadecane is because latent heat of phase change is high, phase transition process is stable, and cyclicity is good, and because its phase transition temperature most connects
Person of modern times's temperature, so as to the advantage for having other phase-change materials incomparable, and becomes the focus of phase-change material research.As solid
Liquid phase-change material, it is in a liquid state after being heated, and easily leakage is impaired.And pass through to prepare a kind of new ZIF-8 claddings n-octadecane phase
Become gas storage material preparation method, problem above is not only solved to a certain extent, also with good hydrogen storage function and should
Use prospect.
The content of the invention
It is an object of the invention to provide a kind of new ZIF-8 coats the preparation method of n-octadecane phase transformation gas storage material, should
Method has itself nontoxic, and reaction is carried out in water environment, without the need for organic solvent, low cost, can be produced in enormous quantities, is tied
Structure is controllable, and encapsulation ratio is high, and good stability is applied widely, and preparation method is simple, and not high to equipment requirement, raw material is easy to get and ring
The advantages of border is friendly.
The above-mentioned purpose of the present invention is achieved through the following technical solutions：Described a kind of new ZIF-8 cladding n-octadecanes
Phase transformation gas storage material is self-assembly of by hydro-thermal method, and with deionized water as solvent, n-octadecane, ZIF-8, SDS are reactant,
Realize that ZIF-8 coats n-octadecane under certain condition；
A kind of above-mentioned new ZIF-8 coats n-octadecane phase transformation gas storage material preparation method, ZIF-8 cladding n-octadecane phase transformations
Gas storage material is prepared by emulsion process, first by lauryl sodium sulfate（SDS, analyzes pure）In being dissolved in deionized water, at a high speed
The n-octadecane for melting is slowly added under stirring（NOD）, for a period of time, SDS wraps up scattered NOD droplets, then for emulsification
Zinc nitrate is slowly added to, after slow stirring it is dissolved, adsorbed on SDS surfaces by the sucking action of opposite charges, add two
Methylimidazole, forms organic metal framework structure, and by vibrating cooling, suction filtration, deionized water is repeatedly washed, centrifugation, very
Sky is dried, the class flower pattern nanostructured phase transformation gas storage material changeable so as to prepare a kind of structure, with the change of reaction condition, shape
Into fancy structure, class petal that the structure of each fancy, the such as hexagon ZIF-8 of two dimension, the hexagon ZIF-8 of two dimension are arranged out
Deng concrete preparation process is as follows：
（1）SDS is dissolved in deionized water, concentration is 2-50 mg/mL, ultrasonic 5 min water-bath 300- at 40-70 DEG C
1000 rpm magnetic agitation 10-15 min, to being uniformly dispersed；
（2）Take and melt at appropriate NOD, 70-80 DEG C, in being added dropwise over the SDS emulsifying agents of high-speed stirred, bath temperature 70-80
DEG C, 50-60 min are stirred, ultrasonic 10-20 min form uniform oil-in-water（O/W）Emulsification droplet；
（3）Take zinc nitrate to dissolve in 50-60 DEG C of appropriate deionized water, in being added dropwise to above-mentioned emulsion, 200-1000
Rpm is slowly stirred to 22-30 min, Zn2+With anion surfactant SDS complexings, uniform adsorption is on SDS surfaces；
（4）The methylimidazole for having dissolved in right amount, after stirring a period of time, 50-60 will be added dropwise in above-mentioned mixed solution again
DEG C, vibration, methylimidazole and Zn under 100-300 rpm2+Metallic organic framework is formed, around cladding NOD, fast quickly cooling is taken out
But, vibrate in case and vibrate 18-24 h, suction filtration, 0 DEG C of deionized water is washed for several times, and freeze-drying obtains class flower pattern nanostructured
Phase transformation gas storage material.
Described solvent deionized water can be replaced with organic solvents such as organic solvent methyl alcohol, ethanol.
Described SDS:NOD=1:2-1:20, the change of consumption does not interfere with basic pattern, but to the size of final structure
And the pattern of threadiness ZIF-8 can have an impact.
Described high-speed stirred speed is 1000-3000 rpm, and impact of the rotating speed to material structure is very big, and rotating speed is too small very
Hardly possible forms the material for needing.
Described SDS can be replaced with other anion surfactants such as AESA-70, AES-2EO-70 etc..
Described ZIF-8:N-octadecane=1:5-1:20, the change of consumption can affect pattern, can obtain different petal-shaped.
Described zinc nitrate is 1 with the mol ratio of methylimidazole:1, the phase-change material for obtaining is easy to removal of impurities, mitigates suction filtration
Burden.
Described oscillatory process is 8 ~ 24h, and time different product yield is variant.
The present invention has advantages below：（1）The reaction mechanism of the present invention is oil phase（N-octadecane）Instill water and mutually realize bag
Wrap up in, a kind of new ZIF-8 is then self-assembly of with ZIF-8 and wraps up n-octadecane phase-change material, with very high heat resistance.
（2）The present invention using the organic ligand such as oxygen-containing, nitrogen and transition metal ions self assembly coordination polymer and
N-octadecane is self-assembly of（MOFs ）, it is to avoid the addition of other toxic chemicals, the pollution to environment is reduced, and
Course of reaction is easily controlled.
（3）Hydrogen storage effect of the present invention is good, and by the manipulation of simple temperature and rotating speed the organic gold of assembling guiding is capable of achieving
The synthesis of category framework compound, course of reaction is easily controlled, and agglomerated prod surface ZIF-8 is evenly distributed, and encapsulation is high, stability
It is good.
（4）The present invention does not need special chemical reagent, and Technology for Heating Processing is simple, environmental protection, and eventually reduces system
Cause this and process complexity.
Description of the drawings
Fig. 1 is the Flied emission Electronic Speculum pattern that new ZIF-8 prepared by the present invention coats n-octadecane phase transformation gas storage material；
Fig. 2 is the Flied emission under the new ZIF-8 cladding n-octadecane phase transformation gas storage material differential responses times prepared by the present invention
Electronic Speculum pattern.
Specific embodiment
Embodiment one
（1）0.3 g SDS are dissolved in 8-16 ml deionized waters, concentration is 2-50 mg/mL, and ultrasonic 5 min is in 40-70
Water-bath 300-1000 rpm magnetic agitation 10-15 min at DEG C, to being uniformly dispersed；
（2）1.0 ml NOD are taken, is melted at 70-80 DEG C, be added dropwise over the SDS emulsifying agents of 1000-1200 rmp high-speed stirreds
In, 70-80 DEG C of bath temperature stirs 50-60 min, and ultrasonic 10-20 min form uniform oil-in-water（O/W）Emulsify little liquid
Drop；
（3）Take 0.6-0.8 g zinc nitrates to dissolve in 50-60 DEG C of appropriate deionized water, in being added dropwise to above-mentioned emulsion,
200-1000 rpm are slowly stirred to 22-30 min, Zn2+With anion surfactant SDS complexings, uniform adsorption is in SDS tables
Face；
（4）The methylimidazole that 1-3 g has dissolved will be added dropwise in above-mentioned mixed solution again, after stirring 10-20 min, 50-
60 DEG C, vibration, methylimidazole and Zn under 100-300 rpm2+Metallic organic framework is formed, around cladding NOD, takes out quick
18-24 h are vibrated in cooling vibration case, suction filtration, 0 DEG C of deionized water is washed for several times, and freeze-drying obtains class flower pattern nano junction
Structure phase transformation gas storage material.
Embodiment two
（1）0.25 g SDS are dissolved in 8-16 ml deionized waters, concentration is 2-50 mg/mL, and ultrasonic 5 min is in 40-70
Water-bath 300-1000 rpm magnetic agitation 10-15 min at DEG C, to being uniformly dispersed；
（2）1.0 ml NOD are taken, is melted at 70-80 DEG C, be added dropwise over the SDS emulsifying agents of 1000-1200 rmp high-speed stirreds
In, 70-80 DEG C of bath temperature stirs 50-60 min, and ultrasonic 10-20 min form uniform oil-in-water（O/W）Emulsify little liquid
Drop；
（3）Take 0.6-0.8 g zinc nitrates to dissolve in 50-60 DEG C of appropriate deionized water, in being added dropwise to above-mentioned emulsion,
200-1000 rpm are slowly stirred to 22-30 min, Zn2+With anion surfactant SDS complexings, uniform adsorption is in SDS tables
Face；
（4）The methylimidazole that 1-3 g has dissolved will be added dropwise in above-mentioned mixed solution again, after stirring 10-20 min, 50-
60 DEG C, vibration, methylimidazole and Zn under 100-300 rpm2+Metallic organic framework is formed, around cladding NOD, takes out quick
18-24 h are vibrated in cooling vibration case, suction filtration, 0 DEG C of deionized water is washed for several times, and freeze-drying obtains class flower pattern nano junction
Structure phase transformation gas storage material.
Embodiment three
（1）0.2 g SDS are dissolved in 8-16 ml deionized waters, concentration is 2-50 mg/mL, and ultrasonic 5 min is in 40-70
Water-bath 300-1000 rpm magnetic agitation 10-15 min at DEG C, to being uniformly dispersed；
（2）1.0 ml NOD are taken, is melted at 70-80 DEG C, be added dropwise over the SDS emulsifying agents of 1000-1200 rmp high-speed stirreds
In, 70-80 DEG C of bath temperature stirs 50-60 min, and ultrasonic 10-20 min form uniform oil-in-water（O/W）Emulsify little liquid
Drop；
（3）Take 0.6-0.8 g zinc nitrates to dissolve in 50-60 DEG C of appropriate deionized water, in being added dropwise to above-mentioned emulsion,
200-1000 rpm are slowly stirred to 22-30 min, Zn2+With anion surfactant SDS complexings, uniform adsorption is in SDS tables
Face；
（4）The methylimidazole that 1-3 g has dissolved will be added dropwise in above-mentioned mixed solution again, after stirring 10-20 min, 50-
60 DEG C, vibration, methylimidazole and Zn under 100-300 rpm2+Metallic organic framework is formed, around cladding NOD, takes out quick
18-24 h are vibrated in cooling vibration case, suction filtration, 0 DEG C of deionized water is washed for several times, and freeze-drying obtains class flower pattern nano junction
Structure phase transformation gas storage material.
Example IV
（1）0.2g SDS are dissolved in 8-16 ml deionized waters, concentration is 2-50 mg/mL, and ultrasonic 5 min is at 40-70 DEG C
Lower water-bath 300-1000 rpm magnetic agitation 10-15 min, to being uniformly dispersed；
（2）0.6 ml NOD are taken, is melted at 70-80 DEG C, be added dropwise over the SDS emulsifying agents of 1000-1200 rmp high-speed stirreds
In, 70-80 DEG C of bath temperature stirs 50-60 min, and ultrasonic 10-20 min form uniform oil-in-water（O/W）Emulsify little liquid
Drop；
（3）Take 0.6-0.8 g zinc nitrates to dissolve in 50-60 DEG C of appropriate deionized water, in being added dropwise to above-mentioned emulsion,
200-1000 rpm are slowly stirred to 22-30 min, Zn2+With anion surfactant SDS complexings, uniform adsorption is in SDS tables
Face；
（4）The methylimidazole that 1-3 g has dissolved will be added dropwise in above-mentioned mixed solution again, after stirring 10-20 min, 50-
60 DEG C, vibration, methylimidazole and Zn under 100-300 rpm2+Metallic organic framework is formed, around cladding NOD, takes out quick
18-24 h are vibrated in cooling vibration case, suction filtration, 0 DEG C of deionized water is washed for several times, and freeze-drying obtains class flower pattern nano junction
Structure phase transformation gas storage material.
Embodiment five
(1) 0.2 g SDS are dissolved in 8-16 ml deionized waters, concentration is 2-50 mg/mL, and ultrasonic 5 min is in 40-70
Water-bath 300-1000 rpm magnetic agitation 10-15 min at DEG C, to being uniformly dispersed；
（2）0.25 ml NOD are taken, is melted at 70-80 DEG C, be added dropwise over the SDS emulsifying agents of 1000-1200 rmp high-speed stirreds
In, 70-80 DEG C of bath temperature stirs 50-60 min, and ultrasonic 10-20 min form uniform oil-in-water（O/W）Emulsify little liquid
Drop；
（3）Take 0.6-0.8 g zinc nitrates to dissolve in 50-60 DEG C of appropriate deionized water, in being added dropwise to above-mentioned emulsion,
200-1000 rpm are slowly stirred to 22-30 min, Zn2+With anion surfactant SDS complexings, uniform adsorption is in SDS tables
Face；
（4）The methylimidazole that 1-3 g has dissolved will be added dropwise in above-mentioned mixed solution again, after stirring 10-20 min, 50-
60 DEG C, vibration, methylimidazole and Zn under 100-300 rpm2+Metallic organic framework is formed, around cladding NOD, takes out quick
18-24 h are vibrated in cooling vibration case, suction filtration, 0 DEG C of deionized water is washed for several times, and freeze-drying obtains class flower pattern nano junction
Structure phase transformation gas storage material.
Embodiment six
1）0.2 g SDS are dissolved in 8-16 ml deionized waters, concentration is 2-50 mg/mL, and ultrasonic 5 min is at 40-70 DEG C
Lower water-bath 300-1000 rpm magnetic agitation 10-15 min, to being uniformly dispersed；
（2）0.5 ml NOD are taken, is melted at 70-80 DEG C, be added dropwise over the SDS emulsifying agents of 1000-1200 rmp high-speed stirreds
In, 70-80 DEG C of bath temperature stirs 50-60 min, and ultrasonic 10-20 min form uniform oil-in-water（O/W）Emulsify little liquid
Drop；
（3）Take 0.6-0.8 g zinc nitrates to dissolve in 50-60 DEG C of appropriate deionized water, in being added dropwise to above-mentioned emulsion,
200-1000 rpm are slowly stirred to 22-30 min, Zn2+With anion surfactant SDS complexings, uniform adsorption is in SDS tables
Face；
（4）The methylimidazole that 1-3 g has dissolved will be added dropwise in above-mentioned mixed solution again, after stirring 10-20 min, 50-
60 DEG C, vibration, methylimidazole and Zn under 100-300 rpm2+Metallic organic framework is formed, around cladding NOD, takes out quick
18-24 h are vibrated in cooling vibration case, suction filtration, 0 DEG C of deionized water is washed for several times, and freeze-drying obtains class flower pattern nano junction
Structure phase transformation gas storage material.
It is only above that presently preferred embodiments of the present invention is sub, above-mentioned design of the invention, those skilled in the art
Can also to this various modification can be adapted and conversion, for example, the selection of technological parameter such as water and organic solvent and several solvents mixing
The adjustment such as ratio, n-octadecane, the ratio of amount of material of ZIF-8 and lauryl sodium sulfate；Operating condition such as reacts temperature
Degree, the change in reaction time etc..
Claims (8)
1. a kind of new ZIF-8 coats the preparation method of n-octadecane phase transformation gas storage material, it is characterised in that：
Described ZIF-8 cladding n-octadecane phase transformation gas storage materials are prepared by emulsion process, first by lauryl sodium sulfate（SDS,
Analysis is pure）In being dissolved in deionized water, the n-octadecane for melting is slowly added under high velocity agitation（NOD）, emulsification a period of time,
SDS wraps up scattered NOD droplets, is then slowly added into zinc nitrate, dissolves it after slow stirring, by the suction of opposite charges
Draw effect absorption on SDS surfaces, add methylimidazole, form organic metal framework structure, cooled down by vibrating, suction filtration,
Deionized water is repeatedly washed, centrifugation, vacuum drying, the class flower pattern nanostructured phase transformation changeable so as to prepare a kind of structure
Gas storage material, with the change of reaction condition, defines the structure of each fancy, the such as hexagon ZIF-8 of two dimension, the hexagon of two dimension
Fancy structure, class petal that ZIF-8 is arranged out etc., concrete preparation process is as follows：
（1）SDS is dissolved in deionized water, concentration is 2-50 mg/mL, ultrasonic 5 min water-bath 300- at 40-70 DEG C
1000 rpm magnetic agitation 10-15 min, to being uniformly dispersed；
（2）Take and melt at appropriate NOD, 70-80 DEG C, in being added dropwise over the SDS emulsifying agents of high-speed stirred, bath temperature 70-80
DEG C, 50-60 min are stirred, ultrasonic 10-20 min form uniform oil-in-water（O/W）Emulsification droplet；
（3）Take zinc nitrate to dissolve in 50-60 DEG C of appropriate deionized water, in being added dropwise to above-mentioned emulsion, 200-1000
Rpm is slowly stirred to 22-30 min, Zn2+With anion surfactant SDS complexings, uniform adsorption is on SDS surfaces；
（4）The methylimidazole for having dissolved in right amount, after stirring a period of time, 50-60 will be added dropwise in above-mentioned mixed solution again
DEG C, vibration, methylimidazole and Zn under 100-300 rpm2+Metallic organic framework is formed, around cladding NOD, fast quickly cooling is taken out
But, vibrate in case and vibrate 18-24 h, suction filtration, 0 DEG C of deionized water is washed for several times, and freeze-drying obtains class flower pattern nanostructured
Phase transformation gas storage material.
2. a kind of new ZIF-8 according to claim 1 coats the preparation method of n-octadecane phase transformation gas storage material, and it is special
Levy and be：Described solvent deionized water can be replaced with organic solvents such as organic solvent methyl alcohol, ethanol.
3. a kind of new ZIF-8 according to claim 1 coats the preparation method of n-octadecane phase transformation gas storage material, and it is special
Levy and be：Described SDS:NOD=1:2-1:20, the change of consumption does not interfere with basic pattern, but final structure pattern is had
Affect.
4. a kind of new ZIF-8 according to claim 1 coats the preparation method of n-octadecane phase transformation gas storage material, and it is special
Levy and be：Described high-speed stirred speed is 1000-3000 rpm, and impact of the rotating speed to material structure is very big, and rotating speed is too small very
Hardly possible forms the material for needing.
5. a kind of new ZIF-8 according to claim 1 coats the preparation method of n-octadecane phase transformation gas storage material, and it is special
Levy and be：Described SDS can be replaced with other anion surfactants such as AESA-70, AES-2EO-70 etc..
6. a kind of new ZIF-8 according to claim 1 coats the preparation method of n-octadecane phase transformation gas storage material, and it is special
Levy and be：Described ZIF-8:N-octadecane=1:5-1:20, the change of consumption can affect pattern, can obtain different petal-shaped.
7. a kind of new ZIF-8 according to claim 1 coats the preparation method of n-octadecane phase transformation gas storage material, and it is special
Levy and be：Described zinc nitrate is 1 with the mol ratio of methylimidazole:1, the phase-change material for obtaining is easy to removal of impurities, mitigates suction filtration
Burden.
8. a kind of new ZIF-8 according to claim 1 coats the preparation method of n-octadecane phase transformation gas storage material, and it is special
Levy and be：Described oscillatory process is 8 ~ 24h, and time different product yield is variant.
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| CN107098681A (en) * | 2017-06-05 | 2017-08-29 | 安徽省亚欧陶瓷有限责任公司 | It is a kind of can phase-change temperature control ceramic tile and preparation method thereof |
| CN108178120A (en) * | 2017-12-27 | 2018-06-19 | 温州大学 | The pattern of anodic alumina films surface nanometer array and controlled in nanometer confinement space its pattern grow method, application |
| CN108380055A (en) * | 2018-02-28 | 2018-08-10 | 天津大学 | The sodium alginate hybridized film of hollow ZIF-8 nano particles filling and preparation and application |
| CN110776645A (en) * | 2019-08-27 | 2020-02-11 | 浙江工业大学 | Preparation method of ZIF series metal-organic framework with flower cluster-shaped hierarchical structure |
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