CN108707235A - A method of generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ - Google Patents
A method of generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ Download PDFInfo
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Abstract
The invention belongs to field of material synthesis technology, and in particular to a method of generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ.The present invention uses " Interfacial Adsorption-reaction in-situ " method, using dry mycelia thin slice as matrix, it places into after being submerged initially in zinc nitrate solution absorption zinc ion and carries out ultrasonic reaction in 2-methylimidazole solution, the ZIF-8/ mycelia composite materials of load multilayer ZIF-8 are obtained after repeated multiple times.This method can effectively make ZIF-8 uniform loads on matrix, form controllable thin layer, and step is simple, quick, at low cost, application prospect is good.
Description
Technical field
The invention belongs to materials synthesis fields, and in particular to a kind of to be loaded to ZIF-8 using Interfacial Adsorption-reaction in-situ
The method that filamentous fungi hyphal surface forms controllable thin layer.
Background technology
ZIF-8 is a kind of material of novel practical, has very high thermal stability (N2In 550 DEG C) and chemical stability,
Big surface area (BET：~1700m2/ g), it can be used as absorption, sensing, the fields such as catalysis, energy storage and gas separation, in order to more preferable
Ground application ZIF-8, ZIF-8 composite material at home and abroad receives significant attention.
Now, there are many method synthesis ZIF-8 composite materials, be broadly divided into in-situ reaction and mixing casting method.It is in situ
Reaction method is that the raw material for synthesizing ZIF-8 is added into matrix, makes the spontaneous length of ZIF-8 to matrix surface；Mixing casting rule is
ZIF-8 crystal particles after synthesis are uniformly mixed by stirring ultrasound with the matrix that can be dissolved in liquid phase, then are cast to glass
Drying forms mixed substrate membrane containing nano-grade molecular sieve on plate.Wherein, although casting method preparation process is simple, microcosmic regulation and control, ZIF-8 can not be carried out
Particle content should not be too high (generally 10%~30%) so that dispersion can not form continuous multilayer ZIF- after casting in the solution
8, so that ZIF-8 characteristic properties are unable to give full play, if ZIF-8 and ZIF-8 in composite polyimide material is than more loose.
And there are preparation process complexity for in-situ reaction, finishing time is long, and carrier costly (is generally GO, CNT, metal oxygen
Compound etc.), and due to can largely form ZIF-8 by-products in solution, the ZIF-8 payload rates of in-situ synthesis are relatively low,
Multilayer ZIF-8 can not be also formed simultaneously, if ZIF-8 more reunites in ZIF-8/GO composite materials, ZIF-8/Al2O3ZIF-8 in film
It is more loose.So propose it is a kind of it is novel can effectively make ZIF-8 uniform loads on matrix, form the preparation of controllable thin layer
Method is very significant.
Invention content
It is an object of the present invention to be difficult to be formed with conventional method in the load of composite material for current ZIF-8 negative
Uniform continuous multilayer ZIF-8 layers are carried, proposition is a kind of to generate ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ
Method.This method preparation process is simple and quick, it is of low cost, continuous multilayer ZIF-8 layers can be effectively formed.
The purpose of the present invention is what is be accomplished by the following way.
A method of ZIF-8/ mycelia composite materials being generated using Interfacial Adsorption-reaction in-situ, by filamentous fungi mycelia
It places into 2-methylimidazole solution after being submerged initially in zinc solution absorption zinc ion and be obtained by the reaction ZIF-8/ mycelia composite woods
Material.
The method for generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ, by filamentous fungi bacterium
Silk places into the process reacted in 2-methylimidazole solution and is repeated at least once more after being submerged initially in zinc solution absorption zinc ion,
Obtain the ZIF-8/ mycelia composite materials of multilayer ZIF-8 loads.
The method for generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ, by filamentous fungi bacterium
Silk, which is submerged initially in after zinc solution absorption zinc ion, to be placed into the process reacted in 2-methylimidazole solution and repeats 2~5 times, excellent
Choosing is repeated 2 times.
The method for generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ, mycelia is first each time
It immerses zinc solution 2~10min absorption zinc ions and is put into 2-methylimidazole solution to hyphal surface, preferably 10min, then by mycelia
In carry out 2~10min of reaction, preferably 6min.
The method for generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ, the zinc salt packet
It includes：Zinc nitrate, zinc chloride or zinc acetate, preferably zinc nitrate；Three can synthesize, but zinc nitrate is commonplace；Described
Filamentous fungi mycelia includes：One or more of Mucor, aspergillus niger, head mold, mould, preferably Mucor.
The method for generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ, zinc solution and 2-
The solvent of methyl imidazole solution includes methanol.It is not ZIF-8 that other solvents such as water, ethyl alcohol, which are combined to out,.
The mycelia of the method for generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ, addition is dry
Weight：Zinc salt：Zinc salt solvent：2-methylimidazole：The mass volume ratio of the solvent of 2-methylimidazole is (20mg~100mg):
(0.8000g~1.000g):(25mL~35mL)：(0.9000g~1.100g)：(35mL~45mL).Aforementioned proportion is preferred
50mg:0.8925g:30mL：0.9852g：40mL can preferably synthesize ZIF-8/ mycelia composite materials with this condition, use
Material thin degree prepared by 50mg dry mycelial weights is lucky, and blocked up internal layer mycelia can not play a role, destructible when excessively thin synthesis.
The method for generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ, is put into 2- methyl miaows
Ultrasonic reaction is carried out in azoles solution, power is 100~1000w；It is preferred that 800w；The temperature of ultrasonic reaction is no more than 40 DEG C, preferably
20℃.Ultrasonic power is too small can not to be synthesized, and excessive noise is too big, and power is excessively high, and ZIF-8 is likely to be broken.
The described method for generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ, after reaction bacterium
Silk directly takes out, and reuses clear water cleaning and dries 2~6h at 50~80 DEG C, preferably 60 DEG C baking 6h.
The method for generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ, the mycelia after culture
It filters, drying obtains mycelia film for reacting；It is preferred that mycelia drying temperature is 50~80 DEG C, further preferred drying temperature is 60
DEG C, the preferably time is 1min~3min, and further preferred drying time is 2min.It is inadequate not dry or dry degree, in ultrasound
Mycelia can shake scattered in reaction process, can be destroyed.
Beneficial effects of the present invention：
(1) for the present invention in a manner of " Interfacial Adsorption-in-situ reaction ", first absorption has stronger adsorption capacity with filamentous fungi
Then zinc ion reacts in 2-methylimidazole solution, in mycelium surface in-situ preparation ZIF-8, can be effectively prevented from ZIF-8
It generates in the solution so that ZIF-8 payload rates improve, and atom utilization improves.
(2) ZIF-8/ mycelia composite materials of the invention, for ZIF-8 crystal particles diameter about in 50nm or so, process is several
Secondary repeated boad operation achievees the purpose that load layer thickness is controllable.
(3) ZIF-8/ mycelia materials of the invention solve the problems, such as the uniform load of ZIF-8 thin layers, mycelium surface shape
At fine and close ZIF-8 layers.The reason of uniform load, may be facilitated by two aspects, first, Zn ions elder generation uniform adsorption is in mycelium
On, pass through ultrasonic reaction Fast back-projection algorithm ZIF-8 so that ZIF-8 crystal seeds are uniformly adhered to hyphal surface, grow up to be formed again later
ZIF-8 crystal, second is that due to repeating the operation several times so that ZIF-8 can form one layer of ZIF-8 to even compact in hyphal surface
Layer.
(4) ZIF-8/ mycelia composite material of the invention better mechanical property in water, is not easy to scatter, main cause is
ZIF-8 is supported on mycelia so that mycelia mechanical strength improves, and possible cause is after ZIF-8 is supported on hyphal surface, quite
In the intensity for strengthening every root fungus silk, and ZIF-8 is not hydrophilic, can completely cut off contact of the mycelia with water so that mycelia machinery is strong
Degree improves, and is not easy to scatter, and can effectively recycle by simple filtration.The material of preparation stirs not cracky in water, bears to stir
Rotor speed is mixed up to 1000rpm.
(5) existing other mycelia composite materials are such as：PmPD/ mycelia, generated time do not include follow-up probably in 6h
Oxidant need to be uninterruptedly added in cleaning, when synthesis；For another example：A kind of biological composite membrane materials of CN201610036944-, modified suction
Attached the effect is unsatisfactory, and modifying process is complicated；The ZIF-8/ mycelia composite material preparation process of the present invention is simple, at low cost,
Speed is fast.Existing other mycelia composite materials mainly utilize the characteristic that can disperse in water of mycelia, and when use need to keep mycelia
The finished product of moisture state, preparation can not be dried, and otherwise can influence dispersion performance, therefore the shipping storage of product is very inconvenient.This
The ZIF-8/ mycelia composite materials of invention, using the characteristic of its microscopic fibers shape, are not stranded above using dry mycelia as carrier
It disturbs.Product of the present invention need to only be applied in the liquid phase, and product itself is drying regime, and when use is put into solution, and without using
The dispersibility of mycelia, reaction terminate also to be still sheet, are easy to transport, the recycling separation after preserving and reacting.
(6) ZIF-8/ mycelia materials of the invention, are reacted, it was found that ZIF-8 is on mycelia interface by repeated boad
Growth course, the course that ZIF-8 is supported on mycelia are that larger particle is first slowly formed on surface, after particle can not be grown again
It is grown along hyphal surface, until being paved with entire hyphal surface, then forms one layer of ZIF-8 on the surface being paved with and (subsequently may be used
To increase thickness and the uniformity by repeated boad), Fig. 1 a are examined, 1b has found that ZIF-8 is easily formed in the crook of mycelia,
Cause ZIF-8 particles herein more than smooth hyphal surface, thus it is speculated that ZIF-8 first should have the coarse place of gauffer formation and length in advance
Greatly, other positions are extended to again later.The present invention approximately passes through 3 loads in mycelium surface, can form dense uniform
The ZIF-8 thin layers of mycelium overall surface can be covered, thickness of thin layer is about 40~60nm, and ZIF-8 can be increased by continuing load
The thickness of thin layer.
The filamentous fungi mycelia that the present invention selects includes Mucor, aspergillus niger, head mold, mould, not necessarily emphasizes it is certain
The special bacterial strain of kind, the conventional bacterial strain of the filamentous fungi of these types.
Description of the drawings：
Fig. 1 a~d are the scanning electron microscope (SEM) photographs of ZIF-8/ mycelia composite materials prepared by 1-4 of the embodiment of the present invention；
Fig. 1 a are the material that reaction is once prepared, and the ZIF-8 number of particles and density on mycelia are minimum, and ZIF-8 is the most
It is sparse；
Fig. 1 b are the material for reacting secondary preparation, and ZIF-8 particles are distributed on mycelia in large area, however still have facet
Product is to have ZIF-8 loads；
Fig. 1 c are the material that reaction is prepared three times, are distributed one layer of fine and close ZIF-8 completely on mycelia；
Fig. 1 d are to react four materials prepared, and on mycelia other than being distributed one layer of fine and close ZIF-8, also another layer is dilute
Thin ZIF-8 is formed thereon.
Fig. 2 is the scanning electron microscope (SEM) photograph of ZIF-8/ mycelia composite materials prepared by the embodiment of the present invention 5；
Fig. 3 is the scanning electron microscope (SEM) photograph of ZIF-8/ mycelia composite materials prepared by the embodiment of the present invention 6.
Specific implementation mode：
With specific embodiment, the invention will be further described below, but can't form limitation of the present invention.
Embodiment 1
Potato culture medium is prepared, the potato for taking 200g to remove the peel, about 10min is boiled in chopping into the water, until glass bar can be used
It breaks, is poured into 1L measuring cups with filtered through gauze after slightly cold, and moisture in soil dynamic test is back-outed easily, 20g glucose, 0.5g is added
Magnesium sulfate and 1.0g potassium dihydrogen phosphates, are settled to 1L, 5 conical flasks are poured into after stirring evenly, each about 200mL, is used in combination sealed membrane
It seals, is put into 115 DEG C of autoclave, sterilize 15min, obtains fluid nutrient medium.With the inoculum concentration of culture volume 2% by concentration
106~107Mucor (Mucormucedo (Linnaeus) Fresenius, deposit number CCTCC AF 93229) bacterium solution of a/ml
It is seeded in fluid nutrient medium and cultivates, it is 30 DEG C to be subsequently placed in temperature, the constant temperature oscillation case culture that rotating speed is 160r/min 3 days；
5mL bacterium solutions (a concentration of 10g/L) volume is pipetted with 5mL liquid-transfering guns, vacuum filtration film forming is put into 60 DEG C of baking ovens and dries 2min dry weights
50mg weighs 0.9852g 2-methylimidazoles and is dissolved in 40mL methanol, and 0.8925g zinc nitrates are dissolved in 30mL methanol, first by dry mycelia
Thin slice, which is put into zinc nitrate solution, impregnates 10min, picks up rear methanol rinses with tweezers, places into 2-methylimidazole solution and carry out
Ultrasound synthesis instrument, power 800w, normal-temperature reaction 10min are obtained material and are pressed from both sides out with tweezers, cleaned with clear water, and at 60 DEG C
6h is dried, obtains ZIF-8/ mycelia materials, as shown in Figure 1a.
Embodiment 2
In embodiment 1 " dry mycelia thin slice to be put into zinc nitrate solution and impregnates 10min, picking up rear methanol with tweezers moistens
Wash, place into 2-methylimidazole solution progress ultrasound synthesis instrument, power 800w, normal-temperature reaction 10min, obtain material with
Tweezers press from both sides out, are cleaned with clear water, " the step of be repeated once, at 60 DEG C dry 6h, obtain ZIF-8/ mycelia materials, as shown in Figure 1 b.
Embodiment 3
With embodiment 1 " dry mycelia thin slice is put into zinc nitrate solution and impregnates 10min, rear methanol rinses are picked up with tweezers,
Progress ultrasound synthesis instrument in 2-methylimidazole solution is placed into, power 800w, normal-temperature reaction 10min obtain material with tweezer
Sub-folder goes out, and is cleaned with clear water, " the step of repeat it is secondary, at 60 DEG C dry 6h, obtain ZIF-8/ mycelia materials, as illustrated in figure 1 c.
Embodiment 4
In embodiment 1 " dry mycelia thin slice to be put into zinc nitrate solution and impregnates 10min, picking up rear methanol with tweezers moistens
Wash, place into 2-methylimidazole solution progress ultrasound synthesis instrument, power 800w, normal-temperature reaction 10min, obtain material with
Tweezers press from both sides out, are cleaned with clear water, " the step of in triplicate, at 60 DEG C dry 6h, obtain ZIF-8/ mycelia materials, as shown in Figure 1 d.
Embodiment 5
It weighs 0.8253g 2-methylimidazoles and is dissolved in 40mL methanol, 0.9439g zinc nitrates are dissolved in 30mL methanol, first by 50mg
Dry mycelia thin slice, which is put into zinc nitrate solution, impregnates 2min, picks up rear methanol rinses with tweezers, places into 2-methylimidazole solution
Middle progress ultrasound synthesis instrument, power 800w, normal-temperature reaction 2min are obtained material and are pressed from both sides out with tweezers, cleaned with clear water, 60
DEG C dry 6h, obtain ZIF-8/ mycelia materials, see Fig. 2.
Embodiment 6
It weighs 0.9784g 2-methylimidazoles and is dissolved in 40mL methanol, 1.0869g zinc nitrates are dissolved in 30mL methanol, first by dry bacterium
Silk thin slice is put into zinc nitrate solution and impregnates 5min, and rear methanol rinses are picked up with tweezers, place into 2-methylimidazole solution into
Row ultrasound synthesis instrument, power 600w, normal-temperature reaction 5min are repeated twice, and are obtained material and are pressed from both sides out with tweezers, clear with clear water
It washes, and dries 6h at 60 DEG C, obtain ZIF-8/ mycelia materials, see Fig. 3.
Embodiment 7
Under room temperature, the ZIF-8/ aspergillus nigers composite material prepared with embodiment 2 is 100mg/L to containing Pb ion concentrations
Solution 20mL is adsorbed, and 0.0110g composite materials (not crushing) are added, and solution filtering, filter are carried out after 4h is adsorbed at 30 DEG C
Pb ion concentrations are used in liquid is measured with inductively coupled plasma atomic emission spectrometry (ICP), filtered Pb ion concentrations
For 12.97mg/L, filter liquor concentration is measured as 91.79mg/L before adsorbing, and Pb removal rates reach 85.87%, and adsorbance reaches
78.82mg/g。
Claims (10)
1. a kind of method generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ, which is characterized in that will be Filamentous
Hypha,hyphae places into 2-methylimidazole solution after being submerged initially in zinc solution absorption zinc ion and carries out that ZIF-8/ bacterium are obtained by the reaction
Wire composite material.
2. the method according to claim 1 for generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ,
Be characterized in that, filamentous fungi mycelia is submerged initially in after zinc solution absorption zinc ion place into 2-methylimidazole solution carry out it is anti-
The process answered is repeated at least once more, and obtains the ZIF-8/ mycelia composite materials of multilayer ZIF-8 loads.
3. the method according to claim 2 for generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ,
Be characterized in that, filamentous fungi mycelia is submerged initially in after zinc solution absorption zinc ion place into 2-methylimidazole solution carry out it is anti-
The process answered repeats 2~5 times, is preferably repeated 2 times.
4. according to claim 1 or 2 or 3 generate ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ
Method, which is characterized in that mycelia is submerged initially in 2~10min of zinc solution and adsorbs zinc ion to hyphal surface, preferably time each time
Range 10min, then mycelia is put into 2-methylimidazole solution and carries out 2~10min of reaction, preferably time range 6min.
5. the method according to claim 1 for generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ,
It is characterized in that, the zinc salt includes：Zinc nitrate, zinc chloride or zinc acetate, preferably zinc nitrate；The filamentous fungi mycelia
Including：One or more of Mucor, aspergillus niger, head mold, mould, preferably Mucor.
6. the method according to claim 1 for generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ,
It is characterized in that, the solvent of zinc solution and 2-methylimidazole solution includes methanol.
7. it is compound that utilization Interfacial Adsorption-reaction in-situ according to claims 1 or 2 or 3 or 5 or 6 generates ZIF-8/ mycelia
The method of material, which is characterized in that the dry mycelial weight of addition：Zinc salt：Zinc salt solvent：2-methylimidazole：2-methylimidazole it is molten
The mass volume ratio of agent is (20mg~100mg):(0.8000g~1.000g):(25mL~35mL)：(0.9000g~
1.100g)：(35mL~45mL)；The preferred 50mg of aforementioned proportion:0.8925g:30mL：0.9852g：40mL.
8. the method according to claim 1 for generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ,
It is characterized in that, is put into 2-methylimidazole solution and carries out ultrasonic reaction, power is 100~1000w；It is preferred that 800w；Ultrasonic reaction
Temperature be no more than 40 DEG C, preferably 20 DEG C.
9. the side for generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ according to claim 1 or 8
Method, which is characterized in that mycelia directly takes out after reaction, reuses clear water cleaning and dries 2~6h at 50~80 DEG C, excellent
Select 60 DEG C of baking 6h.
10. the method according to claim 1 for generating ZIF-8/ mycelia composite materials using Interfacial Adsorption-reaction in-situ,
It is characterized in that, the mycelia after culture filters, drying obtains mycelia film for reacting；It is preferred that mycelia drying temperature is 50~80
DEG C, further preferred drying temperature is 60 DEG C, and the preferably time is 1min~3min, and further preferred drying time is 2min.
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