CN110479112A - A kind of preparation method of infiltrating and vaporizing membrane - Google Patents
A kind of preparation method of infiltrating and vaporizing membrane Download PDFInfo
- Publication number
- CN110479112A CN110479112A CN201810458895.1A CN201810458895A CN110479112A CN 110479112 A CN110479112 A CN 110479112A CN 201810458895 A CN201810458895 A CN 201810458895A CN 110479112 A CN110479112 A CN 110479112A
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- framework compound
- infiltrating
- stephanoporate framework
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- membrane
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- 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
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
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- 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
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0013—Casting processes
-
- 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
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- 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
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- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a kind of preparation methods of infiltrating and vaporizing membrane, belong to technical field of function materials.Prepared sizes are in nanoscale, submicron order or micron-sized stephanoporate framework compound particle first, in a solvent by the dispersion of stephanoporate framework compound particle, it is then added in Polymer Solution, is film-made after mixing, mixed substrate membrane containing nano-grade molecular sieve is obtained after drying, is used for infiltration evaporation.The stephanoporate framework compound is porous aromatic skeleton compound, porous covalent organic framework compound, its biggish aperture and strong-hydrophobicity, be conducive to improve dissolution and diffusion selectivity of the organic matter in film, while improving flux, selectivity and the membrane stability of infiltrating and vaporizing membrane.
Description
The invention belongs to technical field of function materials.
Background technique
Infiltration evaporation (Pervaporation) is a kind of liquid separation technology of great competitive advantage.Liquid mixture exists
Film surface selective absorption dissolution, spread in film, finally film downstream side vaporize, using different component absorption, dissolution and
Difference in diffusion process and realize separation.Compared with conventional separation techniques, infiltration evaporation have low energy consumption, pollute small, equipment
Simply, the advantages that easy to operate.
In infiltration evaporation, traditional macromolecule infiltrating and vaporizing membrane leads to selective reduction because of plasticizing effect.In high score
The advantages of inorganic filler obtains mixed substrate membrane containing nano-grade molecular sieve, has both two kinds of materials is added in son, the stability and permeance property of film can be improved.
However, compatibility is poor between inorganic filler and macromolecule, permeation flux is caused to be difficult to improve simultaneously with separation factor.
Summary of the invention
It is an object of the invention to overcome conventional inorganic fillers, using porous aromatic skeleton compound, covalently have
Machine framework compound prepares mixed-matrix infiltrating and vaporizing membrane as filler.Porous aromatic skeleton compound (Porous
Aromatic Frameworks, PAFs), it is that the porous material constituted is covalently attached by rigid aromatic ring, low with skeletal density,
The advantages that molecule and structure are adjustable, specific surface area is high, surface is easy to functionalization, thermal stability and chemical stability are excellent.Covalently
Organic framework compounds (COFs) are formed by organic molecule covalent bond, have molecule it is easily designed cut out, structure is adjustable, be easy to
The advantages that functional modification, high stability.Porous aromatic skeleton compound and covalent organic framework compound hydrophobicity are strong, aperture
It is larger, it is good with polymer-polymer miscibility, be conducive to the infiltration evaporation performance and stability for improving film, particularly suitable for Organic substance in water
Removal.
The principle of technical solution of the present invention is: prepared sizes are in nanometer, sub-micron or micron-sized stephanoporate framework first
Polymer beads in a solvent by the dispersion of stephanoporate framework compound particle are added in Polymer Solution, are film-made after mixing,
Mixed substrate membrane containing nano-grade molecular sieve is obtained after drying, is separated for infiltration evaporation.Porous aromatic skeleton compound and covalent organic framework compound
Biggish aperture and strong-hydrophobicity are conducive to improve dissolution and diffusion selectivity of the organic matter in film, while improving infiltration vapour
Change flux, selectivity and the membrane stability of film.
A kind of preparation method of infiltrating and vaporizing membrane, it is characterised in that: prepared sizes are in nanometer, sub-micron or micron order first
Stephanoporate framework compound particle, by stephanoporate framework compound particle dispersion in a solvent, be then added in Polymer Solution,
It is film-made after mixing, obtains mixed substrate membrane containing nano-grade molecular sieve after dry, be used for infiltration evaporation.The stephanoporate framework compound is porous virtue
Fragrant framework compound, porous covalent organic framework compound.In the preparation of stephanoporate framework compound, a small amount of surface-active is added
Agent obtains the particle of nanometer or sub-micron.The solvent of dispersing cellular skeleton compounds composition granule it is identical as high molecular solvent or
The two is dissolved each other.The infiltrating and vaporizing membrane is for dehydration of organic solvent, Organic substance in water removal, organic matter/organic matter separation.Institute
The surfactant of addition is dissolved in or is partially soluble in reaction dissolvent.
Detailed description of the invention
Fig. 1: PAF-56 particle electron micrograph；
Fig. 2: PAF-11 particle electron micrograph.
Specific embodiment
Below with reference to embodiment, technical scheme of the present invention will be further described.
The preparation of embodiment 1:PAF-56/ dimethyl silicone polymer (PDMS) mixed-matrix infiltrating and vaporizing membrane
The Cyanuric Chloride that 56ml contains surfactant Span-80 is added dropwise in the para-terpheny solution of 0.014mol/L
In solution (solvent is chloroform), 1.3g AlCl is added while stirring3, after being heated to reflux 5h, it is cooled to room temperature, crosses diafiltration
Decontamination is washed away, the dry 12h at 80 DEG C, acquisition brown PAF-56 powder, 0.83 micron of partial size (Fig. 1).It takes a certain amount of
PAF-56 is dispersed in normal heptane, is added in the n-heptane solution of PDMS, stirs 2h, a certain amount of positive silicic acid second is added later
Ester and dibutyl tin dilaurate.By casting solution on Kynoar (PVDF) ultrafiltration membrane knifing, after natural drying at room temperature, set
Dry 4h, obtains PAF-56/PDMS mixed substrate membrane containing nano-grade molecular sieve in 80 DEG C of vacuum ovens, and the n-butanol aqueous solution for 4% permeates
Vaporization separation.When PAF-56 additive amount is 2.5wt%, the permeation flux and separation factor of mixed substrate membrane containing nano-grade molecular sieve are respectively 1906g m- 2h-1With 48.4,66% and 183% has been respectively increased compared with PDMS blank film.
The preparation of embodiment 2:PAF-11/PDMS mixed-matrix infiltrating and vaporizing membrane
The 4,4'- biphenyl hypoboric acid of four (4- bromophenyl) methane of 248.04mg and 0.78mmol is added to 12mL's
In DMF, then solution of potassium carbonate, a small amount of surface active agent tween -80 and the 45mg that 1.5mL concentration is 2mol/L is added in degassing
Tetrakis triphenylphosphine palladium, degassing, mixture is heated for 24 hours under the conditions of 150 DEG C, is filtered after being cooled to room temperature, wash, vacuum
It is dried to obtain PAF-11 powder, 350 nanometers of partial size (Fig. 2).PDMS is stirred to 4h dissolution in normal heptane, certain mass is added
Then ethyl orthosilicate and dibutyl tin dilaurate is added in the stirring of PAF-11 normal heptane dispersion liquid into solution, stirring 6h is extremely
Silicone rubber crosslinking to certain viscosity, then by casting solution on PVDF basement membrane knifing, film is placed in draught cupboard 14h, later by it
Dry 4h, obtains PAF-11/PDMS mixed substrate membrane containing nano-grade molecular sieve, for 4% n-butanol water under the conditions of being placed in a vacuum drying oven 80 DEG C
The separation of solution infiltration evaporation.When PAF-11 mass fraction is 3%, separation factor 14.025, permeation flux is
2255.83g m-2h-1, compared with blank PDMS film, 40.7% and 10.8% has been respectively increased.
Claims (6)
1. a kind of preparation method of infiltrating and vaporizing membrane, it is characterised in that: prepared sizes are in nanoscale, submicron order or micron first
The stephanoporate framework compound particle of grade in a solvent by the dispersion of stephanoporate framework compound particle is then added to Polymer Solution
In, it is film-made after mixing, obtains mixed substrate membrane containing nano-grade molecular sieve after dry, be used for infiltration evaporation.
2. the method according to claim 1, it is characterised in that: the stephanoporate framework compound is porous aromatic skeleton chemical combination
Object, porous covalent organic framework compound.
3. the method according to claim 1, it is characterised in that: in the preparation of stephanoporate framework compound, a small amount of surface-active is added
Agent obtains the particle of nanometer or sub-micron.
4. the method according to claim 1, it is characterised in that: the solvent of dispersing cellular skeleton compounds composition granule with it is high molecular molten
Agent is identical or both to dissolve each other.
5. the method according to claim 1, it is characterised in that: the infiltrating and vaporizing membrane in dehydration of organic solvent, water for having
The removal of machine object, organic matter/organic matter separation.
6. according to the method in claim 3, it is characterised in that: the surfactant being added, which is dissolved in or is partially soluble in, reacts molten
Agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810458895.1A CN110479112A (en) | 2018-05-15 | 2018-05-15 | A kind of preparation method of infiltrating and vaporizing membrane |
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|---|---|---|---|
| CN201810458895.1A CN110479112A (en) | 2018-05-15 | 2018-05-15 | A kind of preparation method of infiltrating and vaporizing membrane |
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| CN110479112A true CN110479112A (en) | 2019-11-22 |
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| CN201810458895.1A Pending CN110479112A (en) | 2018-05-15 | 2018-05-15 | A kind of preparation method of infiltrating and vaporizing membrane |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112915810A (en) * | 2021-01-26 | 2021-06-08 | 廖威明 | Pollution-resistant oxygen-permeable film material and preparation method thereof |
| CN113509847A (en) * | 2021-04-27 | 2021-10-19 | 北京工业大学 | Method for preparing porous nano particle/polydimethylsiloxane membrane by spreading on water surface |
-
2018
- 2018-05-15 CN CN201810458895.1A patent/CN110479112A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112915810A (en) * | 2021-01-26 | 2021-06-08 | 廖威明 | Pollution-resistant oxygen-permeable film material and preparation method thereof |
| CN113509847A (en) * | 2021-04-27 | 2021-10-19 | 北京工业大学 | Method for preparing porous nano particle/polydimethylsiloxane membrane by spreading on water surface |
| CN113509847B (en) * | 2021-04-27 | 2023-11-03 | 北京工业大学 | Method for preparing porous nanoparticle/polydimethylsiloxane membrane through water surface spreading |
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Application publication date: 20191122 |