CN206244894U - The batch electrochemistry formated device of metal-organic framework materials - Google Patents
The batch electrochemistry formated device of metal-organic framework materials Download PDFInfo
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- CN206244894U CN206244894U CN201621258739.3U CN201621258739U CN206244894U CN 206244894 U CN206244894 U CN 206244894U CN 201621258739 U CN201621258739 U CN 201621258739U CN 206244894 U CN206244894 U CN 206244894U
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Abstract
The utility model is related to a kind of electrochemistry formated device, and in particular to a kind of electrochemistry formated device of metal-organic framework materials.The device includes reaction tank body (1), product groove (2), sieves (3), backflow pool (4), wherein, it is provided with through hole fixture (6) and offers the clamping groove plate (7) of conduit (10) in reaction tank body (1), and is fastened on positive plate and minus plate in the conduit of clamping groove plate (7) (10).By the quantity for adjusting conduit (10), multi-group electrode reaction can simultaneously be carried out, batch synthesis metal-organic framework materials, solution must not in batches prepare the problem of metal-organic framework materials, the purity and yield of product are improved, the design of backflow pool (4) enables reaction medium to reuse, and reduces production cost, reduces environmental pollution.
Description
Technical field
The utility model is related to a kind of electrochemistry formated device and method, and specifically a kind of batch synthesis metal is organic
The electrochemistry formated device of framework material, and the method for synthesizing metal-organic framework materials with described device.
Background technology
Metal-organic framework materials are led to by the organic ligand of inorganic metal center (metal ion or metal cluster) and bridging
Self assembly interconnection is crossed, a class of formation has the crystalline state porous material of periodic network structure, abbreviation MOFs.Due to MOFs
Material is a kind of Inorganic-Organic Hybrid Material, by inorganic metal ion and organic ligand hybrid combination, so it has inorganic material concurrently
The characteristics of material and organic material, inorganic constituents makes it have fixed duct and specific function, and organic principle then makes it possess more
Big specific surface area and the features such as have the easy functionalization of designability, pore size controllability, channel surfaces concurrently.
Chinese patent " a kind of preparation method of nano level metal organic framework material " (Authorization Notice No. 102617646B)
Disclosed in the preparation method of nano level metal organic framework material include slaine, organic ligand in a solvent, it is appropriate to add
Alkali to increase organic ligand solubility in a solvent so that accelerate MOFs nucleation obtain nanoscale MOFs materials, be prepared into
The specific surface area of the nanoscale MOFs materials for arriving is big, and carbon dioxide adsorption ability is strong.
Chinese patent application (application number 201310428964.1) " metal-organic framework materials, its preparation method and its use
Metal-organic framework materials preparation method disclosed on the way " is：Slaine, organic ligand and solvent are loaded into cup in Teflon,
Then cup in Teflon is placed in iron cup, then iron cup is put into pyroreaction is carried out in high temperature furnace, belong to traditional molten
Agent hot preparation method.
Chinese patent application (application number 201410766174.9) " preparations and application of a kind of metal-organic framework materials "
In disclose using hydro-thermal method or heating reflux method synthesis MOF (Fe) material.Hydro-thermal method need in reactor pyroreaction, and
Hydrofluoric acid is used, the method has power consumption greatly, the shortcoming strong to the corrosivity of equipment.
The method of conventional synthesis MOFs materials has the hot method of hydrothermal/solvent, diffusion method, mechanical milling method, microwave to close at present
Into method and ultrasonic etc., these methods exist to varying degrees HTHP highly energy-consuming, synthesis technique it is complicated, to reaction
The problems such as equipment and environmental requirement harshness, low production efficiency.Electrochemical method for synthesizing is a kind of normal temperature and pressure, environmental protection, height
The synthetic method of efficiency, but it is very big skillfully to grasp its technique difficulty.Chinese patent 1886536B discloses a kind of crystallization, more sky
Metal-organic framework materials electrochemical preparation method, but its yield can only achieve a gram level, and and not disclosed specific conjunction
Into device, the utility model devises a set of easily and efficiently electrochemistry formated device, can realize batch synthesis MOFs materials.
Utility model content
The utility model solve technical problem be：Synthesis MOFs materials often use hydrothermal synthesis method, and it needs HTHP, height
Power consumption, synthesis technique are complicated, harsh to consersion unit and environmental requirement, low production efficiency, and yield is also very low, can only achieve gram
Level (g) production.Prior art discloses electrochemistry formated know-why, but without specific device.
The purpose of this utility model is to design a set of dress for easily and efficiently synthesizing MOFs materials using electrochemical method
Put, not only reduces cost, moreover it is possible to which quick, the synthesis metal-organic framework materials monocrystalline of high-purity, yield can reach feather weight
(kg), while realizing the recycling of reaction medium, reducing energy consumption.
Specifically, in view of the shortcomings of the prior art, the utility model provides following technical scheme：
On the one hand, the utility model provides a kind of electrochemistry formated device of metal-organic framework materials, including reaction
Pond body 1 and product groove 2, the device are additionally provided with sieves 3 and backflow pool 4 below product groove 2, wherein, in reaction tank body 1
Inside it is provided with through hole fixture 6 and offers the clamping groove plate 7 of conduit 10, and is fastened on the positive plate in the conduit 10 of clamping groove plate 7
And minus plate.
Preferably, reaction tank body 1 and product groove 2 are connected as one, and through hole fixture 6 is inserted through reaction tank body 1
Enter into product groove 2.
Preferably, the side of the clamping groove plate 7 is fixed on through hole fixture 6, and the quantity of clamping groove plate 7 is at least 3.
Preferably, each clamping groove plate 7 is uniformly distributed centered on through hole fixture 6, and the conduit 10 of the top of each clamping groove plate 7 is distributed
Identical, the quantity of conduit 10 is (3n-1), and n is the group number and at least 1 of electrode reaction.
Preferably, each conduit 10 on clamping groove plate 7 is used to snap in positive plate, minus plate or insulating barrier, each conduit 10
Spacing is 0.5-30mm.
Preferably, each conduit 10 on clamping groove plate 7 is used to snap in positive plate, minus plate or insulating barrier, each conduit 10
Spacing is 1-10mm.
Preferably, two adjacent on clamping groove plate 7 to snap in positive plate identical with the spacing of conduit 10 of minus plate.
Preferably, product groove 2 is in funnel-form, and lower end is provided with plastic piston 9, and sieves 3 is positioned over the top of backflow pool 4, mistake
Screen 3 and backflow pool 4 are arranged at the lower section of reaction tank body 1 independently of reaction tank body 1, and the side wall of backflow pool 4 is provided with hole.
Preferably, be provided with pump in backflow pool 4, return duct 8 via the hole from the intercalation reaction pond body 1 of backflow pool 4, mistake
Screen 3 is the screen cloth of 100-300 mesh.
Preferably, described device also includes outside support 5.
Preferably, the insulating barrier is glass or ceramics, more preferably glass.
Preferably, the positive plate and minus plate being fastened in the conduit 10 of clamping groove plate 7 are same metal, and the metal is selected from
One kind in zinc, copper, manganese, iron, cobalt, nickel, chromium, zirconium, aluminium and titanium, preferably zinc, copper or cobalt.
On the other hand, the utility model is additionally provided and closed using the electrochemistry formated device of aforementioned metal organic framework material
Into the method for metal-organic framework materials, its synthesis step includes：Positive plate, minus plate are snapped in into conduit 10, adds reaction to be situated between
Matter, switches on power, and starts reaction, and product accumulation to product groove 2 retains product by sieves 3, and reaction medium enters backflow pool
4。
Preferably, 2 groups or more than 2 groups cell reactions are carried out, insulating barrier is snapped in toward the conduit 10 is interior.
Preferably, the insulating barrier is glass or ceramics, preferably glass.
Preferably, reaction medium is led back into reaction tank body 1 via return duct 8 by opening the pump in backflow pool 4.
Preferably, the positive plate and minus plate are same metal, selected from zinc, copper, manganese, iron, cobalt, nickel, chromium, zirconium, aluminium and
One kind in titanium, more preferably zinc, copper or cobalt.
Preferably, the reaction medium is the mixture that conducting salt is formed with reactant and solvent.
Preferably, the conducting salt be inorganic acid, sulfonic acid, phosphonic acids, boric acid, alkoxy sulfonic acid, the salt of sulfonamide, quaternary ammonium from
Son or protonation amine in one or more；Reactant is organic ligand compound, including glyoxaline compound, preferably 2- first
Base imidazoles, 2- ethyl imidazol(e)s or benzimidazole；Carboxylic acid compound, preferably terephthalic acid (TPA), M-phthalic acid or equal benzene front three
Acid；Reaction dissolvent is one or more in N,N-dimethylformamide, ethanol, methyl alcohol, dimethyl sulfoxide, tetrahydrofuran and water.
Preferably, by weight, the concentration of conducting salt is 0.1-6.0%, preferably 1.0%-2.0%；Organic ligand chemical combination
The concentration of thing is 0.5-15%, preferably 2.5%-5.0%.
Preferably, the electrical potential difference between positive plate and minus plate is 1.5-30v.
Compared with prior art, the beneficial effects of the utility model are：There is provided can efficiently, batch, inexpensively close
Into the electrochemistry formated device of high purity metal organic framework material, solve the problems, such as that MOFs materials can not be prepared in batches.This
Outward, the abundant recycling of solution, reduces the environmental pollution that organic solvent is caused, and realizes low energy consumption.
Brief description of the drawings
Fig. 1 is the apparatus structure schematic diagram for synthesizing MOFs materials described in embodiment one in batches, wherein 1- reaction tanks body, 2-
Product groove, 3- sieves, 4- backflow pools, 5- outside supports, 6- through hole fixtures, 7- clamping groove plates, 8- return ducts, 9- pistons, groove
Road 10；
Fig. 2 is profiles of the Fig. 1 in A-A ＇ positions；
Fig. 3 is profiles of the Fig. 1 in B-B ＇ positions；
Fig. 4 is the XRD of the ZIF-8 of the synthesis of embodiment two；
Fig. 5 is the SEM figures of the ZIF-8 of the synthesis of embodiment two；
Fig. 6 is the infrared figure of the ZIF-8 of the synthesis of embodiment two；
Fig. 7 is the XRD of the ZIF-8 of the synthesis of embodiment three；
Fig. 8 is the SEM figures of the ZIF-8 of the synthesis of embodiment three；
Fig. 9 is the infrared figure of the ZIF-8 of the synthesis of embodiment three；
Figure 10 is the XRD of the ZIF-67 of example IV synthesis；
Figure 11 is the SEM figures of the ZIF-67 of example IV synthesis；
Figure 12 is the infrared figure of the ZIF-67 of example IV synthesis；
Figure 13 is the XRD of the ZIF-67 of the synthesis of embodiment five；
Figure 14 is the SEM figures of the ZIF-67 of the synthesis of embodiment five；
Figure 15 is the infrared figure of the ZIF-67 of the synthesis of embodiment five.
Specific embodiment
The utility model provides the electrochemistry formated device that a kind of batch synthesizes MOFs materials, can be sent out in normal temperature and pressure
Raw reaction, energy consumption is low, and synthesis technique is simple, and yield can reach feather weight, and reaction medium can be recycled, and be reduced to environment
Pollution, reduces cost.
In a kind of preferred embodiment of the present utility model, there is provided a kind of batch synthesizes the device of MOFs materials, its
Structure composition includes：Reaction tank body 1, product groove 2, sieves 3, backflow pool 4, outside support 5, through hole fixture 6 and open up
There is the clamping groove plate 7 of conduit 10.
Wherein, sieves 3 and backflow pool 4 are located at the lower section of product groove 2, and are not attached to product groove 2；Reaction tank body 1
It is connected as one with product groove 2, outside support 5 fixes reaction tank body 1, through hole fixture 6 is additionally provided with reaction tank body 1
With the positive plate and minus plate for offering the clamping groove plate 7 of conduit 10 and be fastened in the conduit 10 of clamping groove plate 7.
Wherein, the positive plate and minus plate for participating in electrochemical reaction are identical metallic plate, the anode in each group electrolytic cell
Plate is identical with the spacing of minus plate, i.e., the electrode spacing of each Battery pack for carrying out electrolytic cell reaction simultaneously is identical.
Wherein, through hole fixture 6 inserts product groove 2 through reaction tank body 1；The side of clamping groove plate 7 is fixed on through hole and consolidates
Determine on part 6, clamping groove plate 7 is uniformly distributed centered on through hole fixture 6, the quantity of conduit 10 on each clamping groove plate 7 is identical, distribution
It is identical.Contain (3n-1) individual conduit 10 on each clamping groove plate 7, wherein n represents the group number of electrode reaction, n >=1.Snap in for electricity
After the positive plate and minus plate or insulating barrier of pole reaction, multi-turn sheaf space structure is formed in reaction tank body 1.
The opposite side of clamping groove plate 7 can be fixed on the inwall of reaction tank body 1, it is also possible to do not fixed.When clamping groove plate 7
When opposite side is not fixed, clamping groove plate 7 is integrated with through hole fixture 6, can be detached from reaction tank body 1, while in reaction
The engaging part matched with clamping groove plate 7 is set on pond body 1 and the joint face of product groove 2；When using, through hole will be fixed on and fixed
The bottom of the clamping groove plate 7 on part 6 snaps in the engaging matched with clamping groove plate 7 located at reaction tank body 1 and the joint face of product groove 2
Part.
Wherein, the lower end of reactive tank 2 is provided with plastic piston 9, after product is accumulated, opens piston 9, and product is filtered
Sieve 3 is retained, and reaction medium enters backflow pool 4, opens the pump in backflow pool 4, the reaction for reclaiming backflow pool 4 by return duct 8
Medium leads back to reaction tank body 1, realizes that solution is reused, sustained response.
The batch of the utility model design synthesizes the electrochemistry formated device of MOFs materials, is set by clamping groove plate 7
Several conduits 10, snap in the positive plate and minus plate for participating in cell reaction, and after the insulating barrier that each Battery pack is separated,
Many Circle Structures are formed in reaction tank body 1, multi-group electrode reaction can be simultaneously carried out, the yield for synthesizing MOFs reaches feather weight, real
Now batch synthesis metal-organic framework materials.
In another preferred embodiment of the present utility model, the utility model provides a kind of using batch synthesis
The electrochemistry formated device of MOFs materials includes the method that synthesizes MOFs materials, key step：By positive plate, minus plate and
The insulating barrier selected as needed snaps in conduit 10, adds reaction medium, switches on power, and starts reaction, product accumulation to product
Thing groove 2, product is retained by sieves 3, and reaction medium enters backflow pool 4.Wherein, 2 groups or 2 groups are carried out with Top electrode when simultaneously
, it is necessary to snap in insulating barrier in conduit 10 between the battery lead plate of each group electrode reaction during reaction；The reaction medium of addition is
Conducting salt and organic ligand compound are dissolved in the mixture formed after reaction dissolvent；Additional power source is provided between positive plate and minus plate
Electrical potential difference, number range is 1.5-30v.Product opens piston 9 after the accumulation of product groove 2, and product is by 3 sections of sieves
Stay, reaction medium enters backflow pool 4, open the pump in backflow pool 4, the reaction medium that will be reclaimed in backflow pool by return duct 8
Reaction tank body 1 is led back to, realizes that solution is reused, sustained response.
Wherein, positive plate is identical with the material of minus plate, is metal, and anode dissolves or part during this method
Dissolving, belongs to " sacrificial anode ".The preferred zinc of electrode material, copper and cobalt in the utility model, the preferred glass of insulating barrier.Insulation
Dividing plate separates each group electrode, forms multiple independent electrolytic cells, while there is cell reaction, does not influence each other.Positive plate, the moon
Pole plate and insulating barrier are snapped in after each conduit 10 in clamping groove plate 7, form many Circle Structures, make full use of reaction tank body
1 space, realizes multi-group electrode simultaneous reactions, output increased to feather weight.
Wherein, reaction medium includes conducting salt, reactant and solvent.
Wherein, the conducting salt described in reaction medium is inorganic acid, sulfonic acid, phosphonic acids, boric acid, alkoxy sulfonic acid, sulfonamide
Salt, quaternary ammonium ion or protonation amine in one or more, the ammonium salt for preferably protonating.
Wherein, the reactant described in reaction medium is organic ligand compound, including imidazoles and carboxylic acid compound,
It is preferred that 2-methylimidazole, 2- ethyl imidazol(e)s benzimidazole, terephthalic acid (TPA), M-phthalic acid and trimesic acid.
Wherein, the solvent described in reaction medium is DMF, ethanol, methyl alcohol, dimethyl sulfoxide, tetrahydrochysene furan
Mutter and one or more in water.
Wherein, in the procedure of synthesis MOFs materials, by adjust voltage, electric current, conductive salinity and species and
Reaction dissolvent can improve the yield and purity of product.Specifically, response parameter is：Voltage swing between battery lead plate is 1.5-
30v, conductive salinity is 0.1-6.0%, and the concentration of organic ligand is 0.5-15%.Closed with electrochemistry described in the utility model
Synthesize MOFs materials into device, yield can reach feather weight.
MOFs materials batch electrochemistry formated device of the present utility model is further illustrated below by specific embodiment
And synthetic method.
In following embodiment, the producer and specification of agents useful for same and equipment are as shown in Table 1 and Table 2.
The utility model of table 1 is raw materials used and company-information
| Title | Purity/composition | Producer |
| 2-methylimidazole | Analysis is pure | Lark prestige |
| Methyltributylammonichloride chloride | Analysis is pure | Chemical Reagent Co., Ltd., Sinopharm Group |
| Zine plate | 99.98% | Lark prestige |
| Cobalt plate | 99.98% | Lark prestige |
| Ethanol | Analysis is pure | Beijing Chemical Plant |
The information of the utility model device therefor of table 2
Embodiment one
A kind of device of preferred batch electrochemistry formated MOFs materials of the present utility model is as shown in figure 1, described device
Including following units：Reaction tank body 1, product groove 2, sieves 3, backflow pool 4, outside support 5, through hole fixture 6, clamping groove plate
7, the conduit 10 on return duct 8, piston 9 and clamping groove plate 7.
Wherein, reaction tank body 1 is cylindrical shape, is connected as one with funnelform product groove 2, in " pencil stub " shape, instead
The product generated in pond body 1 is answered to be directly entered product groove 2.
Wherein, through hole fixture 6 is glass cylinder, and the side of clamping groove plate 7 is fixed on through hole fixture 6, totally 3 draw-in grooves
Plate 7 is mutually the distribution of hexagonal angle degree；Clamping groove plate 7 is glass plate, and 5 conduits 10 are contained in its top, and the spacing of each conduit 10 is 10mm；It is logical
Hole fixture 6 is placed in the center of reaction tank body 1, and opposite side and the inwall of reaction tank body 1 of clamping groove plate 7 are fixed, so that
Structure in reaction tank body 1 is fixed, after so snapping in the battery lead plate or insulation board of electrolytic cell reaction, in reaction tank body 1
Each part will not drift about.
It should be noted that, when the radius of reaction tank body 1 is much larger than the radius of through hole fixture 6 and the width of clamping groove plate 7
During sum, the opposite side of clamping groove plate 7 is not fixed on the inwall of reaction tank body 1, but by reaction tank body 1 and product
The engaging part matched with clamping groove plate 7 is set on the interface that groove 2 connects, clamping groove plate 7 and through hole fixture 6 are fixed on instead
Answer in pond body 1, in not use device, the clamping groove plate 7 and through hole fixture being connected as one can be from reaction tank bodies 1
Detach dismounting.
The insulating barrier for participating in the positive plate of electrode reaction, minus plate and separating electrolytic cell is cylindrical shape, successively
Snapped in the conduit 10 on draw-in groove 7, same positive plate, minus plate or insulating barrier need to protect when conduit 10 are snapped in
Card snaps in the identical conduit 10 on 3 clamping groove plates 7 simultaneously, that is, ensure that same positive plate, minus plate or insulating barrier lead to relatively
Hole fixture 6 is in identical radius, thereby guarantees that the same group of anode of electrode reaction is consistent with negative electrode spacing.
The top of clamping groove plate used 7 is uniformly provided with 5 conduits 10 in the present embodiment, centered on through hole fixture 6, from it is inner to
It is outer to be sequentially clamped in positive plate, minus plate, insulating barrier, positive plate and minus plate, form two groups of electrolytic cells.Positive plate and minus plate
It is positive plate in identical metallic plate, and two groups of electrolytic cells identical with the spacing of minus plate.
The material of reaction tank body 1 and product groove 2 is glass, and the side material of sieves 3 is stainless steel, and mesh screen is nylon
Net, screen cloth is 100 mesh, and diameter and the diameter of backflow pool 4 of sieves 3 match, i.e., sieves 3 can just be stuck in backflow pool 4
Upper end, independently of reaction tank body 1 and product groove 2.The solution flowed out from product groove 2 by after sieves 3, product quilt
It is trapped on screen cloth, reaction medium flows into backflow pool 4.
It should be noted that, the effect of sieves 3 is retention product, and the area of screen cloth can be greater than, equal to or less than backflow
The cross-sectional area in pond 4, as long as sieves 3 is fixed on into the upper end of backflow pool 4 when product is collected, realizes filtering function.
A small-sized reflux pump is placed with backflow pool 4, pump is connected with return duct 8, pump provides power by returning in backflow pool 4
The reaction medium of receipts leads back to reaction tank body 1 via return duct 8.
Embodiment two
Using electrochemistry formated device synthetic zeolite imidazate frame structure material ZIF-8 described in embodiment one, specific step
Suddenly include：
1) positive plate and minus plate are the zine plate of cylindrical shape, and insulating barrier is cylindric glass partition, by positive plate,
Minus plate and glass partition are sequentially clamped in each conduit, and wherein glass partition is located at the 3rd conduit, two groups of electrolytic cells are separated；
2) closure piston 9, add reaction medium, and the reaction medium is 1.5% conducting salt trimethyl chlorination
The mixed solution that the ethanol solution (2.5%) of ammonium and 2-methylimidazole is formed, cumulative volume is 25L.
3) switch on power, the voltage set between battery lead plate is 5v, starts stirring, rotating speed 300rpm；
4) product of generation is accumulated in product groove 2；
5) piston 9 is opened, product and system solution flow through sieves 3, and product is trapped within screen cloth, solution enters backflow
Pond 4；
6) reflux pump being placed in backflow pool 4 is opened, solution leads back to reaction tank body 1 through return duct 8；
7) product is collected, ethanol is used：Water is 1:The solution of 1 (v/v) is washed 3 times；
8) product dries 2-3h, yield 0.49kg, yield 98.0% at room temperature.
Shown in the corresponding chemical equation of above-mentioned synthetic reaction such as formula (1)-(3)：
Anode reaction：Zn→Zn2++2e-； (1)
Cathode reaction：H-MeIM→MeIM-+H+；2H++2e-→H2(g) (2)
Overall reaction：Zn+2H-MeIM+2H2O→Zn(MeIM)2·2H2O+H2(g) (3)
Structural characterization is carried out to the product ZIF-8 for preparing using XRD, SEM and infrared spectrum analyser, each detection and analysis knot
Fruit sees Fig. 4-6, as a result shows the very pure free from admixtures of ZIF-8 that the utility model method is prepared, and heat endurance is good.
Embodiment three
The present embodiment is with the difference of embodiment two：The composition of reaction medium be 0.1% methyltributylammonichloride chloride with
Voltage between the solution that the ethanol solution of 0.5% organic ligand compound is formed, battery lead plate is 1.5v.
Structural characterization is carried out to the product ZIF-8 for preparing using XRD, SEM and infrared spectrum analyser, each detection and analysis knot
Fruit sees Fig. 7-9, as a result shows the pure free from admixtures of ZIF-8 that the present embodiment is prepared, and heat endurance is good.
Example IV
Specifically walked using electrochemistry formated device synthetic zeolite imidazate frame structure material ZIF-67 described in embodiment one
Suddenly include：
1) positive plate and minus plate are the cobalt plate of cylindrical shape, and insulating barrier is cylindric glass partition, by positive plate,
Minus plate and glass partition are sequentially clamped in each conduit, and wherein glass partition is located at the 3rd conduit, two groups of electrolytic cells are separated；
2) closure piston 9, add reaction medium, and the reaction medium is 1.0% conducting salt cetyl trimethyl hydrogen-oxygen
Change the mixed liquor of ethanol solution (4%) formation of ammonium and 2-methylimidazole, cumulative volume is 25L.
3) switch on power, the voltage set between battery lead plate is 30v, starts stirring, rotating speed 300rpm；
4) product of generation is accumulated in product groove 2；
5) piston 9 is opened, product and system solution flow through sieves 3, and product is trapped within screen cloth, solution enters backflow
Pond 4；
6) reflux pump being placed in backflow pool 4 is opened, solution leads back to reaction tank body 1 through return duct 8；
7) product is collected, ethanol is used：Water is 1:The solution of 1 (v/v) is washed 3 times；
8) product is in drying 1-2h, yield 0.81kg, yield 98.4% at 60 DEG C.
Shown in the corresponding chemical equation of above-mentioned synthetic reaction such as formula (4)-(6)：
Anode reaction：Co→Co2++2e-； (4)
Cathode reaction：H-MeIM→MeIM-+H+；2H++2e-→H2(g) (5)
Overall reaction：Co+2H-MeIM+2H2O→Co(MeIM)2·2H2O+H2(g) (6)
Structural characterization is carried out to the product ZIF-67 for preparing using XRD, SEM and infrared spectrum analyser, each detection and analysis
Result is shown in Figure 10-12, as a result shows the very pure free from admixtures of ZIF-67 that the utility model method is prepared, and heat endurance is good.
Embodiment five
The present embodiment is with the difference of example IV：The composition of reaction medium is 6% DTAC
The solution formed with the ethanol solution of 15% organic ligand compound.
Structural characterization is carried out to the product ZIF-67 for preparing using XRD, SEM and infrared spectrum analyser, each detection and analysis
Result is shown in Figure 13-15, and the pure free from admixtures of ZIF-67 that the present embodiment is prepared, heat endurance is good.
Claims (10)
1. the electrochemistry formated device of a kind of metal-organic framework materials, including reaction tank body (1) and product groove (2), it is special
Levy and be, the device is additionally provided with sieves (3) and backflow pool (4) in product groove (2) lower section, wherein, in reaction tank body (1)
It is provided with through hole fixture (6) and offers the clamping groove plate (7) of conduit (10), and is fastened in the conduit (10) of clamping groove plate (7)
Positive plate and minus plate.
2. the electrochemistry formated device of metal-organic framework materials according to claim 1, it is characterised in that reaction tank body
(1) it is connected as one with product groove (2), through hole fixture (6) is inserted into product groove (2) through reaction tank body (1).
3. the electrochemistry formated device of metal-organic framework materials according to claim 1 or claim 2, wherein, the clamping groove plate (7)
Side be fixed on through hole fixture (6), the quantity of clamping groove plate (7) is at least 3.
4. the electrochemistry formated device of metal-organic framework materials according to claim 3, it is characterised in that each clamping groove plate
(7) it is uniformly distributed centered on through hole fixture (6), the conduit (10) on each clamping groove plate (7) is distributed identical, conduit (10) quantity
It is (3n-1), n is the group number and at least 1 of electrode reaction.
5. the electrochemistry formated device of metal-organic framework materials according to claim 4, it is characterised in that clamping groove plate (7)
On each conduit (10) for snapping in positive plate, minus plate or insulating barrier, the spacing of each conduit (10) is 0.5-30mm.
6. the electrochemistry formated device of metal-organic framework materials according to claim 5, it is characterised in that each conduit (10)
Spacing be 1-10mm.
7. the electrochemistry formated device of metal-organic framework materials according to claim 6, it is characterised in that clamping groove plate (7)
Upper adjacent two to snap in positive plate identical with the conduit of minus plate (10) spacing.
8. the electrochemistry formated device of metal-organic framework materials according to claim 7, it is characterised in that product groove (2)
In funnel-form, lower end is provided with plastic piston (9), and sieves (3) is positioned over backflow pool (4) top, sieves (3) and backflow pool
(4) reaction tank body (1) lower section is arranged at independently of reaction tank body (1), the side wall of backflow pool (4) is provided with hole.
9. the electrochemistry formated device of metal-organic framework materials according to claim 8, wherein, is provided with backflow pool (4)
Pump, via the hole from backflow pool (4) intercalation reaction pond body (1), sieves (3) is the sieve of 100-300 mesh to return duct (8)
Net.
10. the electrochemistry formated device of metal-organic framework materials according to claim 9, it is characterised in that described device
Also include outside support (5).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106498447A (en) * | 2016-11-23 | 2017-03-15 | 北京建筑大学 | The batch electrochemistry formated device and method of metal-organic framework materials |
| CN109183063A (en) * | 2018-11-23 | 2019-01-11 | 南京科技职业学院 | A kind of batch electrochemistry formated device of metal-organic framework materials |
| CN110528019A (en) * | 2019-09-05 | 2019-12-03 | 大连理工大学 | A kind of portable domestic production H2O2Solution containment and method |
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2016
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106498447A (en) * | 2016-11-23 | 2017-03-15 | 北京建筑大学 | The batch electrochemistry formated device and method of metal-organic framework materials |
| CN109183063A (en) * | 2018-11-23 | 2019-01-11 | 南京科技职业学院 | A kind of batch electrochemistry formated device of metal-organic framework materials |
| CN110528019A (en) * | 2019-09-05 | 2019-12-03 | 大连理工大学 | A kind of portable domestic production H2O2Solution containment and method |
| CN110528019B (en) * | 2019-09-05 | 2023-04-18 | 大连理工大学 | Portable household product H 2 O 2 Solution device and method |
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