CN108854569A - A kind of preparation method of metal-organic framework materials MOF loading ZnO scale inhibition ultrafiltration membrane - Google Patents
A kind of preparation method of metal-organic framework materials MOF loading ZnO scale inhibition ultrafiltration membrane Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The present invention relates to a kind of preparation methods of metal-organic framework materials MOF loading ZnO scale inhibition ultrafiltration membrane, belong to inorganic/organic hybrid separation technology field, include the following steps：Using metal salt and ligand as raw material, MOF is prepared under hydrothermal reaction condition, MOF and zinc salt mixing roast obtain MOF loading ZnO, MOF loading ZnO is mixed with membrane material, prepares casting solution, and casting solution prepares MOF loading ZnO scale inhibition ultrafiltration membrane using a variety of methods.Specifically using one kettle way up to MOF loading ZnO, production process is simple, and operation is easy.It is 80~90% to the anti-adhesion of the bacterium being isolated from waste water using above-mentioned MOF loading ZnO ultrafiltration membrane bacteriostasis property with higher；In addition, the anti-tartar ultrafiltration membrane have it is good be separated by filtration performance, to the rejection of bovine serum albumin 95% or more；It can be stabilized in air and water；Recyclable regenerative；It is environmental-friendly, it is non-corrosive.
Description
Technical field
The invention belongs to inorganic/organic hybrid separation technology fields, and in particular to a kind of metal-organic framework materials MOF is negative
Carry the preparation method and applications of ZnO scale inhibition ultrafiltration membrane.
Background technique
ZnO doping ultrafiltration membrane is known as antibacterial film, they can be made up of various techniques.CN201710974986.6
Disclose a kind of method and apparatus of PVDF/ZnO piezoelectricity ultrafiltration membrane coupling high-level oxidation technology advanced treatment of waste water, PVDF/ZnO
Piezoelectricity ultrafiltration membrane realizes automatic cleaning action under AC power source effect, and membrane filtration technique is overcome to cannot be removed effectively small molecule dirt
The problem of dye object and high-level oxidation technology are unable to the efficient oxidation macromolecule contaminant.CN105833742A is in dopen Nano ZnO
The preparation of modified PVDF ultrafiltration membrane and one text of characteristic research are prepared for the PVDF ultrafiltration membrane of dopen Nano ZnO, and research finds doping
The PVDF ultrafiltration membrane hydrophily of nano-ZnO improves, and pure water flux increases, and rejection is also improved, the PVDF of dopen Nano ZnO
The excellent performance of ultrafiltration membrane.However, existing inorganic doping film, the problem with the intermiscibility difference of membrane material is to need to solve at present
Certainly the problem of.For MOF loading ZnO preparation PVDF, PS, PES ultrafiltration membrane, there is not pertinent literature to disclose the preparation work at present
Skill.
MOF is metal-organic framework materials（Metal-OrganicFrameworks）Refer to transition metal ions with it is organic
Ligand passes through the crystalline porous material with periodic network structure being self-assembly of.It has high porosity, low-density, big
Specific surface area, duct rule, aperture is adjustable and topological structure diversity and the advantages that Scalability.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation sides of metal-organic framework materials MOF loading ZnO scale inhibition ultrafiltration membrane
Method solves the problems, such as that the intermiscibility of inorganic doping film and membrane material is poor, and ultrafiltration membrane provided by the invention has excellent antibacterial
Adhesion and separating property.
To achieve the above object, the present invention adopts the following technical scheme that：
Using metal salt and ligand as raw material, MOF is prepared under hydrothermal reaction condition, it is negative to obtain MOF for MOF and zinc salt mixing roast
ZnO is carried, the MOF of loading ZnO and PVDF, PE, PES are dispersed or dissolved in solvent, corresponding loading ZnO is prepared
MOF scale inhibition ultrafiltration membrane.
A kind of preparation method of metal-organic framework materials MOF loading ZnO scale inhibition ultrafiltration membrane, specifically comprises the following steps：
（1）Metal salt is reacted to obtain required MOF material with decanedioic acid, P-hydroxybenzoic acid or 1,3,5- benzenetricarboxylic acid；
（2）MOF material is put into ultrasonic disperse in water and alcohol solvent, zinc acetate solution, stirring one are added dropwise into above-mentioned solution
Roast is carried out after the section time（10 h of heating reaction at 150-230 DEG C）, promote the MOF nano particle of loading ZnO to generate, from
Heart separation, is dried for standby；
（3）MOF nano material, membrane material and the perforating agent of the loading ZnO of drying are dissolved in organic solvent by a certain percentage, magnetic
Power is stirred until homogeneous, stable casting solution, then stands casting solution, ultrasound carries out deaeration processing；Finally phase is caused with non-solvent
Ultrafiltration membrane needed for partition method is made.
Step（1）Described in metal salt be molysite, aluminium salt, magnesium salts or silver salt, metal salt and decanedioic acid, P-hydroxybenzoic acid
Or the molar ratio of 1,3,5- benzenetricarboxylic acid is 0.1:1~3:1.
Step（1）In reaction temperature be 130 DEG C ~ 200 DEG C.
Step（2）In, the molar ratio of MOF and zinc acetate is 100:1~100:40.
Step（3）In, the MOF nano material of loading ZnO and the mass ratio of membrane material are 1:100~10:100.
Step（3）In, one of membrane material PVDF, PE, PES, PSF, organic solvent are dimethyl acetamide, membrane material
The mass ratio of material and organic solvent is 1:10~3:10.
Step（3）In, the casting film temperature of casting solution is 20~100 DEG C, and the casting film time is 5~24 h.
Remarkable advantage of the invention is：
The problem of the intermiscibility of inorganic doping film and membrane material difference is current problem to be solved.
Ultrafiltration membrane provided by the invention has excellent antibacterial adhesion and separating property.
Membrane material includes that MOF loads zinc oxide, loads zinc oxide antibacterial ultrafiltration membrane antibacterial with higher using above-mentioned MOF
Adhesion.In addition, the ultrafiltration membrane is separated by filtration performance with good；It can be stabilized in air and water；It is recycled again
It is raw；It is environmental-friendly, it is non-corrosive.The experimental results showed that：Ultrafiltration membrane provided by the invention to the anti-adhesion of waste water bacterium be 80~
90%, to the rejection of bovine serum albumin 95% or more.
For the present invention compared with direct ZnO doping ultrafiltration membrane, the dispersion performance of ZnO is more preferable, sees Fig. 3 Zn-ef ficiency EDS map.
Detailed description of the invention
Fig. 1 is 1 ultrafiltration membrane antibacterial of case study on implementation（Staphylococcus aureus）Adhesion property photo, a left side are PVDF ultrafiltration membrane,
The right side is that MOF loads zinc oxide PVDF ultrafiltration membrane；
Fig. 2 is 2 ultrafiltration membrane antibacterial of case study on implementation（Waste water isolated strains）Adhesion property photo, a left side are PVDF ultrafiltration membrane, and the right side is
MOF loads zinc oxide PVDF ultrafiltration membrane；
Fig. 3 is Zn-ef ficiency EDS map on 3 film of case study on implementation.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution is described further, but the present invention is not limited only to this.
Embodiment 1
A kind of preparation method of metal-organic framework materials MOF loading ZnO scale inhibition ultrafiltration membrane, specifically comprises the following steps：
（1）Metal salt is reacted to obtain required MOF material at 130 DEG C with decanedioic acid；The metal salt is Mg（NO3）2·
6H2O, Mg（NO3）2·6H2The molar ratio of O and decanedioic acid is 1.3:1.
（2）MOF material is put into ultrasonic disperse in the water and alcohol solvent of 20ml, zinc acetate is added dropwise into above-mentioned solution
Solution heats 10 h of reaction after stirring a period of time at 150 DEG C, promotes the MOF nano particle of loading ZnO to generate, centrifugation point
From being dried for standby；The molar ratio of MOF and zinc acetate is 100:1.
（3）It is 100 by mass ratio:1:3 molecular weight are that 200,000 g/mol PVDF, MOF load zinc oxide, perforating agent dissolution or divide
It is dispersed in and is made into the PVDF solution that mass fraction is 20% in dimethyl acetamide, be allowed to sufficiently dissolve, filtering removal insoluble matter is de-
It is cured 12 hours in 60 DEG C of thermostatic chambers after bubble, obtains casting solution；With scraper on clean glass plate knifing, later immediately will
Glass plate, which is put into deionized water, carries out inversion of phases, and removal residual solvent is impregnated after inversion of phases is complete, in deionized water, is surpassed
Filter membrane.
The antibacterial Adhesion property of ultrafiltration membrane is tested
This experiment is using staphylococcus aureus as the antibacterial Adhesion property for examining ultrafiltration membrane.
Culture medium prescription used in experiment is as follows：
LB liquid medium：1% tryptone, 0.5% yeast extract, 1% sodium chloride, pH value 7.0；
LB solid medium：1% tryptone, 0.5% yeast extract, 1% sodium chloride, pH value 7.0,1.6% agar powder.
S. aureus Inoculate is in 5 mL LB liquid mediums, at 37 DEG C of temperature, after 5000 rpm shake 1h
Centrifugation, thallus wash centrifugation 3 times with phosphate buffer solution (PBS), are made into containing 106A/mL bacterium solution.In the above-mentioned anti-of 2cm × 2cm
It is inoculated on bacterium ultrafiltration membrane in 20 mL bacterium solutions, 20 min is cultivated in the environment of humidity is 90, with phosphate buffer solution (PBS)
Washing 1 time；Then film is put on LB solid medium.Antibacterial sticks test chart and sees Fig. 1.A left side is blank group in Fig. 1, the right side is real
The antibacterial adhesion test chart of the antibacterial ultrafiltration membrane of the preparation of example 1 is applied, as seen from the figure, case study on implementation has preferable antibacterial adhesiveness
Energy.
Embodiment 2
A kind of preparation method of metal-organic framework materials MOF loading ZnO scale inhibition ultrafiltration membrane, specifically comprises the following steps：
（1）Metal salt is reacted to obtain required MOF material at 150 DEG C with 1,3,5- benzenetricarboxylic acid；The synthetic method is Fe
Powder and nitric acid, hydrofluoric acid, 1,3,5- benzenetricarboxylic acid（BTC）Synthesize MIL-Fe, Fe powder and 1,3,5- benzenetricarboxylic acids（BTC）Mole
Than being 1.58:1.
（2）MOF material is put into ultrasonic disperse in the water and alcohol solvent of 40ml, it is molten that zinc acetate is added dropwise into above-mentioned solution
Liquid heats 10 h of reaction after stirring a period of time at 180 DEG C, promotes the MOF nano particle of loading ZnO to generate, centrifugation point
From being dried for standby；The molar ratio of MOF and zinc acetate is 100:10.
（3）It is 100 by mass ratio:2:3 molecular weight are that 200,000 g/mol PVDF, MOF load zinc oxide, perforating agent dissolution
Or be dispersed in and be made into the PVDF solution that mass fraction is 20% in dimethyl acetamide, it is allowed to sufficiently dissolve, filtering removal is insoluble
It is cured 12 hours in 60 DEG C of thermostatic chambers after object deaeration, obtains casting solution；With scraper on clean glass plate knifing, Zhi Houli
Glass plate is put into deionized water and carries out inversion of phases, removal residual solvent is impregnated after inversion of phases is complete, in deionized water, is obtained
To ultrafiltration membrane.
The antibacterial Adhesion property of ultrafiltration membrane is tested
This experiment is using waste water separation bacterium as the antibacterial Adhesion property for examining ultrafiltration membrane.
Culture medium prescription used in experiment is as follows：
LB liquid medium：1% tryptone, 0.5% yeast extract, 1% sodium chloride, pH value 7.0；
LB solid medium：1% tryptone, 0.5% yeast extract, 1% sodium chloride, pH value 7.0,1.6% agar powder.
Waste water separation bacterium is inoculated in 5 mL LB liquid mediums, at 37 DEG C of temperature, 5000 rpm shake after 12h from
The heart, thallus wash centrifugation 3 times with phosphate buffer solution (PBS), are made into containing 106A/mL bacterium solution.In the above-mentioned antibacterial of 2cm × 2cm
It is inoculated with bacterium solution on ultrafiltration membrane to be inoculated into 20 mL bacterium solutions, cultivates 20 min in the environment of humidity is 90, uses phosphate buffer solution
(PBS) it washs 1 time；Then film is put in 20 min of LB phosphate buffer solution (PBS) ultrasound.Dilution 104After take 100 μ L to be applied to
On LB solid medium, uniformly, 37 DEG C of cultures for 24 hours, count clump count for coating.Antibacterial sticks test result and sees Fig. 2.It is left in Fig. 2
It is the antibacterial adhesion test chart of antibacterial ultrafiltration membrane prepared by embodiment 2 for blank group, the right side, as seen from the figure, case study on implementation group tool
There is good antibacterial Adhesion property.
Embodiment 3
A kind of preparation method of metal-organic framework materials MOF loading ZnO scale inhibition ultrafiltration membrane, specifically comprises the following steps：
（1）Metal salt is reacted to obtain required MOF material at 180 DEG C with P-hydroxybenzoic acid；The metal salt is Mg
(NO3)2·6H20, metal salt and ligand（P-hydroxybenzoic acid）Molar ratio be 3:1.
（2）MOF material is put into ultrasonic disperse in the water and alcohol solvent of 60ml, it is molten that zinc acetate is added dropwise into above-mentioned solution
Liquid heats 10 h of reaction after stirring a period of time at 200 DEG C, promotes the MOF nano particle of loading ZnO to generate, centrifugation point
From being dried for standby；The molar ratio of MOF and zinc acetate is 100:20.
（3）It is 100 by mass ratio:2:3 molecular weight are that 200,000 g/mol PSF, MOF load zinc oxide, perforating agent dissolution
Or be dispersed in and be made into the PS solution that mass fraction is 20% in dimethyl acetamide, it is allowed to sufficiently dissolve, filtering removal insoluble matter
It is cured 12 hours in 60 DEG C of thermostatic chambers after deaeration, obtains casting solution；With scraper on clean glass plate knifing, immediately later
Glass plate is put into deionized water and carries out inversion of phases, removal residual solvent is impregnated after inversion of phases is complete, in deionized water, is obtained
Ultrafiltration membrane.Fig. 3 is shown in the distribution of zinc in ultrafiltration membrane.
Embodiment 4
A kind of preparation method of metal-organic framework materials MOF loading ZnO scale inhibition ultrafiltration membrane, specifically comprises the following steps：
（1）Metal salt is reacted to obtain required MOF material at 200 DEG C with decanedioic acid；The metal salt is Mg（NO3）2·
6H2O, Mg（NO3）2·6H2The molar ratio of O and decanedioic acid is 1.3:1.
（2）MOF material is put into ultrasonic disperse in the water and alcohol solvent of 80ml, it is molten that zinc acetate is added dropwise into above-mentioned solution
Liquid heats 10 h of reaction after stirring a period of time at 230 DEG C, promotes the MOF nano particle of loading ZnO to generate, centrifugation point
From being dried for standby；The molar ratio of MOF and zinc acetate is 100:40.
（3）It is 100 by mass ratio:2:3 molecular weight are that 200,000 g/mol PES, MOF load zinc oxide, perforating agent dissolution
Or be dispersed in and be made into the PES solution that mass fraction is 20% in dimethyl acetamide, it is allowed to sufficiently dissolve, filtering removal insoluble matter
It is cured 12 hours in 60 DEG C of thermostatic chambers after deaeration, obtains casting solution；With scraper, knifing, knife stitch 150 μ on clean glass plate
Glass plate is put into deionized water immediately carries out inversion of phases later by m, and it is residual that removal is impregnated after inversion of phases is complete, in deionized water
Solvent is stayed, ultrafiltration membrane is obtained.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention, for this field skill
For art personnel, it is clear that invention is not limited to the details of the above exemplary embodiments, and without departing substantially from spirit of the invention or
In the case where essential characteristic, the present invention can be realized in other specific forms.Therefore, in all respects, should all incite somebody to action
Embodiment regards exemplary as, and is non-limiting, the scope of the present invention by appended claims rather than on state
Bright restriction, it is intended that including all changes that fall within the meaning and scope of the equivalent elements of the claims in the present invention
It is interior.Any reference signs in the claims should not be construed as limiting the involved claims.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (9)
1. a kind of preparation method of MOF loading ZnO scale inhibition ultrafiltration membrane, which is characterized in that specifically comprise the following steps：
（1）Metal salt is reacted to obtain required MOF material with decanedioic acid, P-hydroxybenzoic acid or 1,3,5- benzenetricarboxylic acid；
（2）MOF material is put into ultrasonic disperse in water and alcohol solvent, zinc acetate solution, stirring one are added dropwise into above-mentioned solution
Roast is carried out after the section time, the MOF nano particle of loading ZnO is promoted to generate, is centrifugated, is dried for standby；
（3）MOF nano material, membrane material and the perforating agent of the loading ZnO of drying are dissolved in organic solvent by a certain percentage, magnetic
Power is stirred until homogeneous, stable casting solution, then stands casting solution, ultrasound carries out deaeration processing；Finally phase is caused with non-solvent
Ultrafiltration membrane needed for partition method is made.
2. a kind of preparation method of MOF loading ZnO scale inhibition ultrafiltration membrane according to claim 1, which is characterized in that step
（1）Described in metal salt be molysite, aluminium salt, magnesium salts or silver salt, metal salt and decanedioic acid, P-hydroxybenzoic acid or 1,3,5- benzene three
The molar ratio of formic acid is 0.1:1 to 3:1.
3. a kind of preparation method of MOF loading ZnO scale inhibition ultrafiltration membrane according to claim 1, which is characterized in that step
（1）In reaction temperature be 130 DEG C ~ 200 DEG C.
4. a kind of preparation method of MOF loading ZnO scale inhibition ultrafiltration membrane according to claim 1, which is characterized in that step
（2）In, the molar ratio of MOF and zinc acetate is 100:1~100:40.
5. a kind of preparation method of MOF loading ZnO scale inhibition ultrafiltration membrane according to claim 1, which is characterized in that step
（2）In, firing temperature is 150-230 DEG C, calcination times 10h.
6. a kind of preparation method of MOF loading ZnO scale inhibition ultrafiltration membrane according to claim 1, which is characterized in that step
（3）In, the MOF nano material of loading ZnO and the mass ratio of membrane material are 1:100~10:100.
7. a kind of preparation method of MOF loading ZnO scale inhibition ultrafiltration membrane according to claim 1, which is characterized in that step
（3）In, one of membrane material PVDF, PE, PES, PSF, organic solvent are dimethyl acetamide, membrane material and organic solvent
Mass ratio be 1:10~3:10.
8. a kind of preparation method of MOF loading ZnO scale inhibition ultrafiltration membrane according to claim 1, which is characterized in that step
（3）In, the casting film temperature of casting solution is 20~100 DEG C, and the casting film time is 5~24 h.
9. MOF loading ZnO scale inhibition ultrafiltration membrane made from preparation method a method as claimed in any one of claims 1-8.
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| CN111034720A (en) * | 2019-12-27 | 2020-04-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of zinc oxide-metal organic framework composite antibacterial material |
| US11254691B1 (en) | 2021-02-22 | 2022-02-22 | Kuwait Institute For Scientific Research | Method for making metal organic frameworks and thin film nanocomposite membranes using the same |
| CN114887494A (en) * | 2022-06-14 | 2022-08-12 | 西北农林科技大学 | Preparation method and application of metal ion leaching-free response release type MIL-53 modified membrane |
| CN117815912A (en) * | 2024-03-05 | 2024-04-05 | 内蒙古森鼎环保节能股份有限公司 | Anti-pollution long-life ultrafiltration membrane material and preparation method thereof |
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Application publication date: 20181123 |