CN111514765A - Preparation method of MIL-101(Fe) -doped straw-based cellulose acetate composite membrane - Google Patents
Preparation method of MIL-101(Fe) -doped straw-based cellulose acetate composite membrane Download PDFInfo
- Publication number
- CN111514765A CN111514765A CN202010353378.5A CN202010353378A CN111514765A CN 111514765 A CN111514765 A CN 111514765A CN 202010353378 A CN202010353378 A CN 202010353378A CN 111514765 A CN111514765 A CN 111514765A
- Authority
- CN
- China
- Prior art keywords
- mil
- cellulose acetate
- preparation
- implementation method
- drying
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920002301 cellulose acetate Polymers 0.000 title claims abstract description 35
- 239000013179 MIL-101(Fe) Substances 0.000 title claims abstract description 26
- 239000010902 straw Substances 0.000 title claims abstract description 26
- 239000012528 membrane Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002131 composite material Substances 0.000 title claims abstract description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 32
- WFDIJRYMOXRFFG-UHFFFAOYSA-N acetic acid anhydride Natural products CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims abstract description 28
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 25
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 17
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 13
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims abstract description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229960000583 acetic acid Drugs 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 229920002678 cellulose Polymers 0.000 claims abstract description 5
- 239000001913 cellulose Substances 0.000 claims abstract description 5
- 239000011521 glass Substances 0.000 claims abstract description 5
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 150000002505 iron Chemical class 0.000 claims abstract description 4
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 90
- 239000000243 solution Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 229920006221 acetate fiber Polymers 0.000 claims description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims 2
- 238000010298 pulverizing process Methods 0.000 claims 1
- 230000002194 synthesizing effect Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 5
- 230000004907 flux Effects 0.000 abstract description 4
- 238000010612 desalination reaction Methods 0.000 abstract description 3
- 238000010335 hydrothermal treatment Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract description 3
- 239000013535 sea water Substances 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract 2
- 238000010306 acid treatment Methods 0.000 abstract 1
- 229910052742 iron Inorganic materials 0.000 abstract 1
- 239000013384 organic framework Substances 0.000 abstract 1
- 239000012621 metal-organic framework Substances 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 238000006640 acetylation reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000004941 mixed matrix membrane Substances 0.000 description 1
- 239000002052 molecular layer Substances 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920005597 polymer membrane Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/08—Polysaccharides
- B01D71/12—Cellulose derivatives
- B01D71/14—Esters of organic acids
- B01D71/16—Cellulose acetate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01D69/12—Composite membranes; Ultra-thin membranes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
Abstract
A preparation method of an MIL-101(Fe) -doped cellulose acetate composite membrane relates to a preparation method of a composite material. The invention comprises the following steps: (1) preparing straw-based cellulose: extracting the straw powder by using a mixed solution of toluene and ethanol; sequentially carrying out alkali treatment and acid treatment on the dry powder; mixing the product with glacial acetic acid, acetic anhydride and sulfuric acid, heating and stirring (recovering glacial acetic acid), washing precipitate, centrifuging and drying to obtain the cellulose acetate. (2) Preparation of MIL-101 (Fe): adding iron salt and terephthalic acid into N, N-dimethylformamide, and performing hydrothermal treatment to obtain yellow powder, namely an MIL-101(Fe) material; MIL-101(Fe) is a typical iron-based organic framework material that helps to improve the performance of cellulose acetate composite films. (3) Preparing a MIL-101(Fe) -doped cellulose acetate composite membrane: MIL-101(Fe) and N, N-dimethylformamide were mixed and dispersed ultrasonically. Adding acetone, polyethylene glycol-400 and cellulose acetate to react for 6 hours at room temperature, defoaming and forming a film on a glass plate. The prepared MIL-101(Fe) -doped cellulose acetate membrane shows higher water flux and salt rejection rate, and has good application prospects in the aspects of high-salinity wastewater and seawater desalination.
Description
Technical Field
The invention relates to a preparation method of an MIL-101(Fe) -doped cellulose acetate composite membrane.
Background
In the 21 st century, the phenomenon of water resource shortage increased with population growth and water pollution aggravation. Sewage reuse and seawater desalination are rapidly becoming the most promising solutions to meet water resource demands. For decades, membrane technology has been widely used in the practice of wastewater reclamation and seawater desalination.
Membrane preparation can use a variety of different raw materials such as metal, ceramic, graphite, glass and polymer powders. In fact, all polymers can be used as barrier material or film material, but their chemical and physical properties are so different that in practice only a limited number thereof can be used. The phase inversion process caused by immersion precipitation is the most common technique for preparing asymmetric polymer membranes; by immersing the substrate in a coagulation bath, the solvent in the casting solution is exchanged with the non-solvent in the precipitation medium, and phase separation occurs. This process produces asymmetric membranes with dense top layers and porous sub-layers, the molecular layer formation can be regulated by controlling many variables in the polymer coating solution, such as composition, coagulation temperature and organic/inorganic additives.
Renewable, biodegradable, and eco-friendly natural polymer materials are receiving wide attention in the field of membrane technology. The Cellulose Acetate (CA) is prepared from cellulose through acetylation reaction, has the characteristics of rich raw materials, wide sources, hydrophilicity, chlorine resistance and the like, and the cellulose acetate membrane prepared from the cellulose acetate has the characteristics of high hydrophilicity, high water flux and the like, which is beneficial to minimizing membrane scaling. Cellulose acetate can improve permeability and selectivity of the membrane compared to other polymers such as polyvinyl alcohol, polyethylene glycol, polyamide, etc., and thus, cellulose acetate membranes are widely used in membrane filtration processes.
In recent years, researchers have utilized novel porous hydrophilic materials, including graphene oxide, carbon nanotubes, Metal Organic Frameworks (MOFs), etc., as additives to improve the performance of membranes. The metal organic frameworks are formed of metal ions or metal groups and organic linkers, and they have permanent porosity, stable frameworks, huge surface area and pore volume, and thus are considered as multifunctional materials for storage, separation, catalysis, and the like. The organic linker gives the MOF a good affinity for the organic polymer, which facilitates the formation of non-covalent bonds between the two. Non-covalent interactions are used to enhance interfacial compatibility, which helps to improve the properties of the membrane active layer without any negative impact on its selectivity. Thus, MOF-based Mixed Matrix Membranes (MMMs) have been extensively studied.
Disclosure of Invention
In conclusion, the invention aims to develop an acid and alkali resistant cellulose acetate membrane with high water flux and salt rejection rate, high mechanical strength: provided herein is a method for preparing an MIL-101(Fe) -doped cellulose acetate film.
The preparation method of the MIL-101(Fe) -doped cellulose acetate membrane comprises the following steps:
firstly, cutting straws into pieces, soaking the cut straws in deionized water, drying the straws, crushing the straws by using a wall breaking machine, sieving the straws, extracting the straws by using a mixed solution of toluene and ethanol, and drying the straws; adding a certain amount of KOH solution into the dried straw powder, stirring, heating to a certain temperature, keeping for 2 hours, cooling to room temperature, centrifuging, and drying. Adding the dried straw powder into an acetic acid solution, stirring, heating to a certain temperature, keeping for 5h, cooling the mixture to room temperature, centrifuging, and drying. The obtained cellulose was mixed with glacial acetic acid, acetic anhydride and sulfuric acid, the mixture was heated with stirring, and glacial acetic acid was recovered. After cooling to room temperature, the precipitate was washed to neutrality, centrifuged and dried.
Secondly, adding FeCl into N, N-Dimethylformamide (DMF)3•6H2O and terephthalic acid (H)2BDC), fully mixing, and carrying out hydrothermal reaction; washing and drying the product after hydrothermal treatment to obtain yellow powder, namely MIL-101 (Fe).
And thirdly, mixing the MIL-101(Fe) obtained in the second step with acetone, performing ultrasonic dispersion, adding DMF (dimethyl formamide), polyethylene glycol-400 and the cellulose acetate obtained in the step 1 into the mixed solution after the dispersion is finished, stirring for 6 hours at room temperature, and forming a film on a glass plate after the mixed solution is defoamed.
Wherein the mass fraction of the KOH solution in the first step is 1-10%; vGlacial acetic acid: VAcetic anhydride: VSulfuric acid=1: 1: 0.1%~1%。
In the second step, the iron salt is FeCl3•6H2O。
Step two m (FeCl)3•6H2O): m(H2BDC): m(DMF)=1: 1: 200~300。
In the third step, the mass fraction of the polyethylene glycol-400 is 1% -10%; the mass fraction of the cellulose acetate is 10-20%.
Drawings
FIG. 1 is a FTIR chart of MIL-101(Fe) -doped cellulose acetate film obtained by practicing the first embodiment.
FIG. 2 is an SEM image of a MIL-101(Fe) -doped cellulose acetate film obtained by practicing the first embodiment.
FIG. 3 is a water flux plot of pure water at standard conditions for MIL-101(Fe) -doped cellulose acetate membranes obtained in accordance with one embodiment of the present invention.
FIG. 4 is a graph of the salt rejection of MIL-101(Fe) -doped cellulose acetate membranes obtained in standard 0.1MNaCI solutions.
Detailed description of the invention
The specific implementation method comprises the following steps:
the preparation method of the MIL-101(Fe) -doped acetate fiber membrane comprises the following steps:
firstly, cutting straws into pieces, soaking the cut straws in deionized water, drying the straws, crushing the straws by using a wall breaking machine, sieving the straws, extracting the straws by using a mixed solution of toluene and ethanol, and drying the straws; adding a certain amount of KOH solution into the dried straw powder, stirring, heating to a certain temperature, keeping for 2 hours, cooling to room temperature, centrifuging, and drying. Adding the dried straw powder into an acetic acid solution, stirring, heating to a certain temperature, keeping for 5 hours, cooling the mixture to room temperature, centrifuging, and drying. The obtained cellulose was mixed with glacial acetic acid, acetic anhydride and sulfuric acid, the mixture was heated with stirring, and glacial acetic acid was recovered. Cooling to room temperature, washing the precipitate to neutrality, centrifuging and drying;
secondly, adding FeCl into DMF3•6H2O and H2BDC, carrying out hydrothermal reaction after fully mixing; washing and drying the product after hydrothermal treatment to obtain yellow powder, namely MIL-101 (Fe);
thirdly, the mixture is preparedMixing MIL-101(Fe) obtained in the step two with acetone, performing ultrasonic dispersion, adding DMF (dimethyl formamide), PEG-400 and cellulose acetate obtained in the step 1 into the mixed solution after dispersion is finished, stirring for 6 hours at room temperature, and forming a film on a glass plate after the mixed solution is defoamed; wherein in the step one, the KOH mass concentration is 1 percent, and V isGlacial acetic acid: VAcetic anhydride: VSulfuric acid=1:1 : 0.1%，m(FeCl3•6H2M (terephthalic acid), m (N, N-dimethylformamide) =1:1: 200, and the mass fraction of PEG-400 is 1%; the mass fraction of the cellulose acetate is 10 percent.
The specific implementation method II comprises the following steps: the first difference between the implementation method and the specific implementation method is that: the mass concentration of KOH in the first step is 2 percent, and the rest is the same as that of the first specific implementation method.
The specific implementation method comprises the following steps: the first difference between the implementation method and the specific implementation method is that: the mass concentration of KOH in the first step is 4%, and the other steps are the same as those of the first specific implementation method.
The specific implementation method four: the first difference between the implementation method and the specific implementation method is that: the mass concentration of KOH in the first step is 6 percent, and the rest is the same as that of the first specific implementation method.
The concrete implementation method comprises the following steps: the first difference between the implementation method and the specific implementation method is that: the mass concentration of KOH in the first step is 8 percent, and the rest is the same as that of the first specific implementation method.
The specific implementation method six: the first difference between the implementation method and the specific implementation method is that: the KOH mass concentration in the first step is 10 percent, and the rest is the same as that of the first specific implementation method.
The specific implementation method is seven: the fourth difference between the implementation method and the specific implementation method is that: in step one, VGlacial acetic acid: VAcetic anhydride:VSulfuric acidAnd =1:1: 0.2%, the other steps being the same as those of the fourth embodiment.
The specific implementation method eight: the fourth difference between the implementation method and the specific implementation method is that: in step one, VGlacial acetic acid: VAcetic anhydride:VSulfuric acidAnd =1:1: 0.4%, the other steps being the same as those of the fourth embodiment.
The specific implementation method comprises the following steps: the implementation method is different from the specific implementation methodThe method comprises the following steps: in step one, VGlacial acetic acid: VAcetic anhydride:VSulfuric acidAnd =1:1: 0.6%, the other steps being the same as those of the fourth embodiment.
The specific implementation method comprises the following steps: the fourth difference between the implementation method and the specific implementation method is that: in step one, VGlacial acetic acid: VAcetic anhydride:VSulfuric acidAnd =1:1: 0.8%, the other steps being the same as those of the fourth embodiment.
The specific implementation method eleven: the fourth difference between the implementation method and the specific implementation method is that: in step one, VGlacial acetic acid:VAcetic anhydride: VSulfuric acidAnd (3) =1:1: 1%, and the other steps are the same as those in the fourth embodiment.
The specific implementation method is twelve: the ninth implementation method is different from the specific implementation method in that: m (FeCl)3•6H2O): m(H2BDC) = m (dmf) =1:1: 220, and the rest is the same as in the specific embodiment nine.
The specific implementation method thirteen is as follows: the ninth implementation method is different from the specific implementation method in that: m (FeCl)3•6H2O): m(H2BDC) = m (dmf) =1:1: 240, and the rest is the same as in the specific embodiment nine.
The specific implementation method is fourteen: the ninth implementation method is different from the specific implementation method in that: m (FeCl)3•6H2O): m(H2BDC) = m (dmf) =1:1: 280, and the rest is the same as in the specific embodiment nine.
The concrete implementation method is fifteen: the ninth implementation method is different from the specific implementation method in that: m (FeCl)3•6H2O): m(H2BDC) = m (dmf) =1:1: 300, and the rest is the same as in the specific embodiment nine.
The specific implementation method is sixteen: the implementation method is different from the specific implementation method by thirteen: PEG-400 mass percent is 2%, and the rest is the same as the specific implementation method thirteen.
The specific implementation method comprises the following steps: the implementation method is different from the specific implementation method by thirteen: PEG-400 mass percent is 4%, and the rest is the same as the specific implementation method thirteen.
The specific implementation method is eighteen: the implementation method is different from the specific implementation method by thirteen: PEG-400 mass percent is 6%, and the rest is the same as the specific implementation method thirteen.
The specific implementation method is nineteen: the implementation method is different from the specific implementation method by thirteen: the mass fraction of PEG-400 is 8%, and the rest is the same as the specific implementation method thirteen.
The specific implementation method twenty: the implementation method is different from the specific implementation method by thirteen: PEG-400 mass percent is 10%, and the rest is the same as the specific implementation method thirteen.
The specific implementation method twenty one: the nineteenth difference between the implementation method and the specific implementation method is that: the mass fraction of cellulose acetate was 12%, and the other steps were the same as those of the nineteen specific embodiments.
The specific implementation method twenty one: the nineteenth difference between the implementation method and the specific implementation method is that: the mass fraction of cellulose acetate was 14%, and the other steps were the same as those of the nineteen specific embodiments.
The specific implementation method twenty one: the nineteenth difference between the implementation method and the specific implementation method is that: the mass fraction of cellulose acetate was 16%, and the other steps were the same as those of the nineteen specific embodiments.
The specific implementation method twenty one: the nineteenth difference between the implementation method and the specific implementation method is that: the mass fraction of cellulose acetate was 18%, and the other steps were the same as those of the nineteen specific embodiments.
The specific implementation method twenty one: the nineteenth difference between the implementation method and the specific implementation method is that: the mass fraction of cellulose acetate was 20%, and the other steps were the same as those of the nineteen specific embodiments.
Claims (7)
1. A preparation method of an MIL-101(Fe) -doped straw-based cellulose acetate composite membrane is characterized by comprising the following steps:
1) preparation of cellulose acetate: cutting straw, soaking in deionized water, drying, pulverizing with wall breaking machine, sieving, extracting with mixed solution of toluene and ethanol, and drying; adding a certain amount of potassium hydroxide solution into the dry straw powder, stirring, heating to a certain temperature, keeping for 2 hours, cooling to room temperature, centrifuging, and drying; adding the dried straw powder into an acetic acid solution, stirring, heating to a certain temperature, keeping for 5 hours, cooling the mixture to room temperature, centrifuging, and drying; mixing the prepared cellulose with glacial acetic acid, acetic anhydride and sulfuric acid, heating and stirring the mixture, and recovering the glacial acetic acid; after cooling to room temperature, the precipitate was washed to neutrality, centrifuged and dried.
2.2) preparation of MIL-101 (Fe): adding iron salt into N, N-dimethylformamide, stirring terephthalic acid, fully mixing, and synthesizing by a hydrothermal method; and (3) washing and drying to obtain yellow powder, namely MIL-101 (Fe).
3.3) preparation of MIL-101(Fe) acetate fiber film: MIL-101(Fe) and N, N-dimethylformamide are mixed and then subjected to ultrasonic dispersion; after the dispersion is finished, adding acetone, polyethylene glycol-400 and cellulose acetate into the N, N-dimethylformamide mixed solution; after stirring at room temperature for 6 hours, the mixture was defoamed and then formed into a film on a glass plate.
4. The preparation method according to claim 1, wherein the mass fraction of the potassium hydroxide solution in the step 1 is 1% -10%; vGlacial acetic acid: VAcetic anhydride: VSulfuric acid=1: 1: 0.1%~1%。
5. The method according to claim 1, wherein the iron salt in step 2 is FeCl3•6H2O。
6. The method according to claim 1, wherein m (FeCl) in step 23•6H2O): m(H2BDC): m(DMF)=1: 1: 200~300。
7. The preparation method according to claim 1, wherein the mass fraction of polyethylene glycol-400 in step 3 is 1% -10%; the mass fraction of the cellulose acetate is 10-20%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010353378.5A CN111514765A (en) | 2020-04-29 | 2020-04-29 | Preparation method of MIL-101(Fe) -doped straw-based cellulose acetate composite membrane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010353378.5A CN111514765A (en) | 2020-04-29 | 2020-04-29 | Preparation method of MIL-101(Fe) -doped straw-based cellulose acetate composite membrane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111514765A true CN111514765A (en) | 2020-08-11 |
Family
ID=71904602
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010353378.5A Pending CN111514765A (en) | 2020-04-29 | 2020-04-29 | Preparation method of MIL-101(Fe) -doped straw-based cellulose acetate composite membrane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111514765A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112430910A (en) * | 2020-10-29 | 2021-03-02 | 武汉轻工大学 | Method for preparing cellulose acetate and P25 porous flexible fibrous membrane by electrospinning, porous flexible fibrous membrane obtained by same and application thereof |
| CN113398771A (en) * | 2021-06-30 | 2021-09-17 | 中国科学院合肥物质科学研究院 | Multi-component bacterial cellulose composite filter membrane and preparation method and application thereof |
-
2020
- 2020-04-29 CN CN202010353378.5A patent/CN111514765A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112430910A (en) * | 2020-10-29 | 2021-03-02 | 武汉轻工大学 | Method for preparing cellulose acetate and P25 porous flexible fibrous membrane by electrospinning, porous flexible fibrous membrane obtained by same and application thereof |
| CN113398771A (en) * | 2021-06-30 | 2021-09-17 | 中国科学院合肥物质科学研究院 | Multi-component bacterial cellulose composite filter membrane and preparation method and application thereof |
| CN113398771B (en) * | 2021-06-30 | 2022-10-25 | 中国科学院合肥物质科学研究院 | Multi-component bacterial cellulose composite filter membrane and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhao et al. | The potential of Kevlar aramid nanofiber composite membranes | |
| CN109092087B (en) | Graphene oxide modified polyamide composite nanofiltration membrane and preparation method thereof | |
| CN103446899B (en) | Organic and inorganic surface chemically-crosslinked alginate-based hybrid hydrogel filter membrane, and preparation method thereof | |
| CN103446898B (en) | Alginate-base organic-inorganic composite hydrogel filtering membrane and preparation method thereof | |
| CN103446897B (en) | Chemical and ionic cross-linked alginate hydrogel flat membrane for filtration and preparation method thereof | |
| CN109289550B (en) | Preparation method and application of anti-pollution polyvinylidene fluoride hybrid ultrafiltration membrane | |
| CN103861472A (en) | Preparation method of amino-modified graphene oxide composite positive permeable film | |
| CN111760461B (en) | Preparation method of polyvinylidene fluoride mixed matrix membrane | |
| CN108246130B (en) | GO/SiO2Preparation method of modified nano composite film | |
| CN110201558B (en) | Large-flux reinforced PVDF unlined ultrafiltration membrane and preparation method thereof | |
| CN110935335B (en) | High-hydrophilicity polymer hybrid membrane and preparation method thereof | |
| CN106621831B (en) | A method of it is quickly nanofiltration membrane by micro-filtration or ultrafiltration membrane converted in-situ | |
| CN110479109B (en) | Preparation method of polyvinylidene fluoride mixed matrix membrane with high flux and strong pollution resistance | |
| CN111514765A (en) | Preparation method of MIL-101(Fe) -doped straw-based cellulose acetate composite membrane | |
| CN101879415A (en) | Method and equipment for preparing ultra-hydrophilic type ultrafiltration membrane | |
| CN102743980A (en) | Manufacture method of polyvinyl chloride panel ultrafiltration membrane | |
| CN107096396A (en) | A kind of polyvinylidene fluoride hollow fiber miillpore filter and preparation method thereof | |
| CN100493689C (en) | Polyaryl ether sulphone compound separation membrane and its preparation method | |
| Miao et al. | Hierarchical aramid nanofibrous membranes from a nanofiber-based solvent-induced phase inversion process | |
| CN116407956A (en) | Polyamide nano composite membrane with high charge distribution pore canal and preparation method thereof | |
| CN104190264A (en) | Preparation method for hollow fiber ultrafiltration membrane with chelation function | |
| CN108479414A (en) | A kind of hollow fibre polymeric membranes, preparation method and its purposes in salt refining | |
| Abbasa et al. | Fabrication of polysulfone/carbon nanospheres ultrafiltration membranes for removing some dyes from aqueous solutions | |
| CN111229059A (en) | Cyclodextrin grafted anglerite nanotube organic solvent nanofiltration membrane and preparation method thereof | |
| CN111013392A (en) | Hybrid ultrafiltration membrane and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20200811 |
|
| WD01 | Invention patent application deemed withdrawn after publication |