CN104607072B - Chitosan-modified mesoporous silicon oxide fills hybridized film and preparation method and application - Google Patents
Chitosan-modified mesoporous silicon oxide fills hybridized film and preparation method and application Download PDFInfo
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- CN104607072B CN104607072B CN201510008419.6A CN201510008419A CN104607072B CN 104607072 B CN104607072 B CN 104607072B CN 201510008419 A CN201510008419 A CN 201510008419A CN 104607072 B CN104607072 B CN 104607072B
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- 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
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- Y02C20/40—Capture or disposal of greenhouse gases of CO2
Abstract
The invention discloses chitosan-modified mesoporous silicon oxide and fill hybridized film, be made up of polyoxyethylene polycaprolactam block copolymer and chitosan-modified mesoporous silicon oxide.Its preparation process includes: prepare chitosan-modified mesoporous silicon oxide；Preparation polyoxyethylene polycaprolactam block copolymer solution；Chitosan-modified mesoporous silicon oxide addition polyoxyethylene polycaprolactam block copolymer solution is prepared casting solution, and final prepared chitosan-modified mesoporous silicon oxide fills hybridized film.The membrane separating property of hybridized film of the present invention is excellent, and preparation method is easily operated, and membrane material used is cheap.It is used for separating CO by this hybridized film2/CH4Gaseous mixture, its CO2Flux is 1835barrer, CO2/CH4Separation factor is 36；For separating CO2/N2Gaseous mixture, its flux is 1943barrer, CO2/N2Separation factor is 85.
Description
Technical field
The present invention relates to a kind of gas separation membrane, particularly relate to a kind of chitosan-modified mesoporous silicon oxide and fill hybridized film
And preparation method and application.
Background technology
Due to greenhouse gases CO2The series of environmental problems that brings of discharge, efficient carbon capture method has caused generation
The extensive concern of various countries of boundary.Compared to the gas separating methods such as traditional absorption process, absorption method and cryogenic separation, membrane separating method
As a kind of novel gas separating method, high with its separation efficiency, energy consumption is low, technique is flexible, equipment is simple, easily operated,
The features such as environmental friendliness are at CO2Trapping field has potential advantage.The kind of gas separation membrane is broadly divided into macromolecule at present
Film, inoranic membrane and hybrid organic-inorganic film.For polymeric membrane, its infiltration coefficient and selectivity are by " tradeoff " effect system
About, i.e. infiltration coefficient increase can cause optionally declining, and vice versa.For inoranic membrane, high infiltration generally can be obtained
Coefficient and high selectivity, but this membrane material is more crisp, be easily generated defect, expensive and be difficulty with industrialization.And select
Prepare hybrid organic-inorganic film as dispersion phase, polymer matrix as continuous phase with inorganic particulate, combine polymeric membrane and
The advantage of inoranic membrane, obtains high osmosis and the selective hybridized film of height while being expected to overcome " tradeoff " effect.At present
Conventional inorganic particulate includes: zeolite, CNT, mesoporous silicon oxide, metal organic knot framework etc..Wherein, mesoporous dioxy
SiClx contains great amount of hydroxy group, bigger specific surface area (> 1000m with its surface2/ g), orderly pore passage structure (1.5-10nm), relatively
Big pore volume (> 0.7cm3/ g) and good mechanical strength and heat stability and obtain extensive concern.
But preparation hybridized film is easily generated the problem such as boundary defect and particle aggregation, have impact on the gas separating property of film.
It is thus typically necessary to surface of inorganic particles to be modified the compatibility improving between inorganic particulate and polymer matrix.Shell gathers
Sugar is as a kind of native biopolymer, and polymer matrix has the preferable compatibility；Containing function bases such as amino on its chain
Group can be as CO2Carrier；It addition, chitosan is a kind of superabsorbent hydrogel, it is possible to absorb substantial amounts of water and water insoluble, water
The raising of content can increase CO2Dissolubility in film.Based on this, select chitosan as the dressing agent of mesoporous silicon oxide, have
Hope the interface compatibility improving between polymer matrix and inorganic particulate, improve CO2The water content of film is improved while vector contg.
Summary of the invention
For prior art, the present invention provides a kind of chitosan-modified mesoporous silicon oxide to fill hybridized film, selects shell to gather
Sugar modifies mesoporous silicon oxide as biopolymer, and the mesoporous silicon oxide after modifying fill to polyoxyethylene-poly-oneself
Lactams block copolymer is prepared hybridized film, it is thus achieved that Thief zone coefficient and the selective CO of height2Separate film.The present invention provides
The preparation process of this hybridized film is simple, and the chitosan-modified mesoporous silicon oxide prepared is filled hybridized film and be may be used for separating
CO2/CH4And CO2/N2Gaseous mixture, under unstripped gas and purge gas humidified condition, has high osmosis and high separation factor.
The chitosan-modified mesoporous silicon oxide of one that the present invention proposes fills hybridized film, this hybridized film thickness 70-105 μ
M, and by the polyoxyethylene that mass fraction is 60-98%-polycaprolactam block copolymer and chitosan-modified meso-porous titanium dioxide
Silicon forms, and in described polyoxyethylene-polycaprolactam block copolymer, polyoxyethylene segment accounts for block copolymer mass fraction
55-60%, polycaprolactam segment accounts for the 40-45% of block copolymer mass fraction.
Above-mentioned chitosan-modified mesoporous silicon oxide fills the preparation method of hybridized film, comprises the following steps:
Step 1, the preparation of chitosan-modified mesoporous silicon oxide:
Step 1-1, to add mass concentration in a container be the cetyl trimethylammonium bromide solution of 0.002g/mL,
Then it is added dropwise over the sodium hydroxide solution of 2.0mol/L so that the concentration of sodium hydroxide is 0.014mol/L, treats that oil bath reaches
80 DEG C are continued stirring 40min, are slowly added dropwise tetraethyl orthosilicate, and tetraethyl orthosilicate is 1.43 times of added sodium hydroxide volume, protects
Stopped reaction after 3h is reacted under the conditions of holding 80 DEG C；Gained solution is carried out sucking filtration, is first washed with deionized 3 times, then uses second
Alcohol washing obtains solid product 1 time；Gained solid product is put in cuvette, the vacuum drying oven of 40 DEG C is dried 48h,
Obtain the mesoporous silicon oxide of band template；
Step 1-2, the mesoporous silicon oxide of the band template weighing step 1-1 gained add in a container, are subsequently adding dense
The volume ratio of hydrochloric acid and methanol, concentrated hydrochloric acid and methanol is 1: 0.06, and the meso-porous titanium dioxide silicon concentration obtaining band template is
The solution of 0.009mg/mL, condensing reflux stirring 48h at temperature 65 DEG C；It is centrifuged gained solution afterwards separating, washes 3
Time, dehydrated alcohol is washed 1 time, after putting into the dry 48h of vacuum drying oven, obtains mesoporous silicon oxide；
Step 1-3, weigh a certain amount of chitosan, this chitosan be dissolved in the glacial acetic acid solution that mass fraction is 5%,
Room temperature mechanical stirring 24h, it is thus achieved that mass fraction is the chitosan solution of 1%；Weigh the mesoporous silicon oxide of step 1-2 gained,
This meso-porous titanium dioxide Si powder is dispersed in ethanol solution, obtains the mesoporous silicon oxide mixture that mass fraction is 1%, super
Sound 15min, and with the glacial acetic acid of pH=4.8 by described mesoporous silicon oxide mixture regulation to pH be 3.5-4.5；The rapidest
The γ of the quality such as addition and mesoporous silicon oxide-glycidyl ether oxygen propyl trimethoxy silicane forms mixture A, and room temperature continues
Stirring 3h；The chitosan solution that volume ratio is 2 times of mesoporous silicon oxide mixture is added in mixture A, 24h is stirred at room temperature,
Centrifugal washing 3 times, washing with alcohol 1 time, after putting into the dry 48h of vacuum drying oven, it is thus achieved that chitosan-modified mesoporous silicon oxide；
The preparation of step 2, polyoxyethylene-polycaprolactam block copolymer solution: in mass ratio 1: (10-50), will be poly-
Oxygen ethylene-polycaprolactam block copolymer adds in the ethanol that mass fraction is 65-75%, at temperature 75-80 DEG C, and backflow
Heat more than 75 DEG C, stir 0.5-4h, make polyoxyethylene-polycaprolactam block copolymer be completely dissolved, obtain mass fraction
For 2-7% polyoxyethylene-polycaprolactam block copolymer solution；
The preparation of step 3, chitosan-modified mesoporous silicon oxide filling hybridized film: in mass ratio 1: the ratio of (100-300)
Example, polyoxyethylene-polycaprolactam that the chitosan-modified mesoporous silicon oxide of gained in step 1 is added step 2 prepared is embedding
In section copolymer solution, stir 5-10h at room temperature, the casting solution of gained is poured on clean glass plate curtain coating, in room temperature
Under dry, be then placed in vacuum drying oven removing the solvent of residual, obtain chitosan-modified mesoporous silicon oxide fill hybridized film.
It is used for separating CO by chitosan-modified mesoporous silicon oxide described above filling hybridized film2/CH4Mixture, its CO2
Flux is 450-1835barrer, CO2/CH4Separation factor is 15-36.This hybridized film can be additionally used in separation CO2/N2Mixture,
CO2Flux is 460-1943barrer, CO2/N2Separation factor is 49-85.
Compared with prior art, preparation method of the present invention is easily operated, and membrane material used is cheap, and membrane separating property is excellent
Different.Chitosan-modified mesoporous silicon oxide is filled and can significantly improve the boundary between polymer matrix and inorganic particulate to film
The face compatibility, improve CO in film2The content of carrier also improves the water content in film, so that permeability of the membrane and separation
Selectivity significantly improves.Other can also be selected CO for chitosan-modified dose used2The functional polymer hydrogel material of carrier,
Such as gelatin, hyaluronic acid and sodium alginate etc..
Accompanying drawing explanation
Fig. 1 is the SEM sectional drawing that the chitosan-modified mesoporous silicon oxide obtained by embodiment 1 fills hybridized film；
Fig. 2 is the SEM sectional drawing that the chitosan-modified mesoporous silicon oxide obtained by embodiment 2 fills hybridized film；
Fig. 3 is the SEM sectional drawing that the chitosan-modified mesoporous silicon oxide obtained by embodiment 3 fills hybridized film；
Fig. 4 is the SEM sectional drawing that the chitosan-modified mesoporous silicon oxide obtained by embodiment 4 fills hybridized film；
Fig. 5 is the SEM sectional drawing filling hybridized film without chitosan-modified mesoporous silicon oxide obtained by comparative example.
Detailed description of the invention
Tell about the detailed content of the present invention by the following examples, it is provided that embodiment is the convenience in order to understand, be definitely not
Limit the present invention.
Embodiment 1: prepare chitosan-modified mesoporous silicon oxide and fill hybridized film.
The thickness of this hybridized film is 85 μm, by the polyoxyethylene that 12.5g mass fraction is 4%-polycaprolactam block altogether
The chitosan-modified mesoporous silicon oxide composition of polymers and 0.05g, in described polyoxyethylene-polycaprolactam block copolymer,
Polyoxyethylene segment accounts for the 60% of block copolymer mass fraction, and polycaprolactam segment accounts for block copolymer mass fraction
40%, the preparation process of this hybridized film is as follows:
Step 1, the preparation of chitosan-modified mesoporous silicon oxide:
Step 1-1, measuring 480ml deionized water, add 1.0g cetyl trimethylammonium bromide, liquid agitation becomes homogeneous
After, it is added dropwise over NaOH solution 3.5ml of 2.0mol/L.Treat that oil bath reaches 80 DEG C and continues stirring 40min, be slowly added dropwise 5ml's
Tetraethyl orthosilicate, under the conditions of keeping 80 DEG C, stops after reaction 3h.After gained solution is carried out sucking filtration, first use 500ml deionized water
Washing, then obtains solid product by 250ml washing with alcohol.Solid product is put in cuvette, the vacuum drying of 40 DEG C
Case is dried 48h, obtains the mesoporous silicon oxide of band template；
Step 1-2, the mesoporous silicon oxide of the band template weighing 5.25g add in container, are subsequently adding the dense of 31.5ml
Hydrochloric acid and 560ml methanol, condensing reflux stirring 48h at temperature 65 DEG C.It is centrifuged gained solution afterwards separating, water afterwards
Wash 3 times to wash 1 time with dehydrated alcohol again, after putting into the dry 48h of vacuum drying oven, obtain mesoporous silicon oxide；
Step 1-3, weighing the chitosan of 2.0g, the mass fraction being dissolved in 200mL is in 5% glacial acetic acid solution, room
Temperature mechanical agitation 24h.Obtain the chitosan solution of 1%.Weigh the meso-porous titanium dioxide Si powder of the above-mentioned acquisition of 0.1g, disperseed
In the ethanol solution of 10mL, ultrasonic 15min, between glacial acetic acid (PH=4.8) regulation to 3.5-4.5.Then it is rapidly added
γ-the glycidyl ether oxygen propyl trimethoxy silicane of 0.1g, room temperature continues stirring 3h.The chitosan solution of 20mL is added mixed
In compound, 24h being stirred at room temperature, centrifugal washing 3 times, washing with alcohol 1 time, after putting into the dry 48h of vacuum drying oven, it is thus achieved that shell gathers
Sugar-modified mesoporous silicon oxide；
Step 2, weigh 0.5g polyoxyethylene-polycaprolactam block copolymer (trade name Pebax 1657), 3.6g
Deionized water and 8.4g dehydrated alcohol add in container, are placed in the water bath with thermostatic control of 80 DEG C, and reflux under stirring 2h, makes block copolymerization
Thing all dissolves, and is then cooled to room temperature standby.
Step 3, chitosan-modified mesoporous silicon oxide fill the preparation of hybridized film: weigh 0.025g chitosan-modified mesoporous
Silicon dioxide adds above-mentioned 12.5g polyoxyethylene-polycaprolactam block copolymer solution, stirs 6h, by the casting solution of gained
Be poured on clean polyfluortetraethylene plate curtain coating, under room temperature, be dried more than 24h, then 45 DEG C, be dried 24h under vacuum condition,
Obtaining thickness is 85 μm hybridized film.Fig. 1 is the SEM sectional drawing of the hybridized film that embodiment 1 prepares.
Under the conditions of room temperature, 1bar, it is used for separating CO by this hybridized film2Volume fraction is the CO of 30%2/CH4Mixing edema caused by disorder of QI
From test, its CO2Infiltration coefficient is 710barrer, CO2/CH4Separation factor is 20；It is used for separating CO by this hybridized film2Volume
Mark is the CO of 10%2/N2Mixed gas separation is tested, its CO2Infiltration coefficient is 770barrer, CO2/N2Separation factor is 57.
Embodiment 2: prepare chitosan-modified mesoporous silicon oxide and fill hybridized film.
The thickness of this hybridized film is 89 μm, by the polyoxyethylene that 12.5g mass fraction is 4%-polycaprolactam block altogether
The chitosan-modified mesoporous silicon oxide composition of polymers and 0.05g, in described polyoxyethylene-polycaprolactam block copolymer,
Polyoxyethylene segment accounts for the 60% of block copolymer mass fraction, and polycaprolactam segment accounts for block copolymer mass fraction
40%, its preparation method the difference is that only with above-described embodiment 1: in step 3, by chitosan-modified mesoporous silicon oxide
Consumption is become 0.05g from 0.025g, finally gives the chitosan-modified mesoporous silicon oxide that thickness is 89 μm homogenizing and fills hydridization
Film.Fig. 2 is the SEM sectional drawing of the hybridized film that embodiment 2 prepares.
Under the conditions of room temperature, 1bar, it is used for separating CO by this hybridized film2Volume fraction is the CO of 30%2/CH4Mixing edema caused by disorder of QI
From test, its CO2Infiltration coefficient is 990barrer, CO2/CH4Separation factor is 24；It is used for separating CO by this hybridized film2Volume
Mark is the CO of 10%2/N2Mixed gas separation is tested, its CO2Infiltration coefficient is 1082barrer, CO2/N2Separation factor is 68.
Embodiment 3: prepare chitosan-modified mesoporous silicon oxide and fill hybridized film.
The thickness of this hybridized film is 96 μm, by the polyoxyethylene that 12.5g mass fraction is 4%-polycaprolactam block altogether
The chitosan-modified mesoporous silicon oxide composition of polymers and 0.075g, in described polyoxyethylene-polycaprolactam block copolymer,
Polyoxyethylene segment accounts for the 60% of block copolymer mass fraction, and polycaprolactam segment accounts for block copolymer mass fraction
40%, its preparation method the difference is that only with above-described embodiment 1: in step 3, by sulfonic acid funtionalized hollow Nano water-setting
Glue consumption is become 0.075g from 0.025g, finally gives the chitosan-modified mesoporous silicon oxide that thickness is 96 μm homogenizing and fills miscellaneous
Change film.Fig. 3 is the SEM sectional drawing of the hybridized film that embodiment 3 prepares.
Under the conditions of room temperature, 1bar, it is used for separating CO by this hybridized film2Volume fraction is the CO of 30%2/CH4Mixing edema caused by disorder of QI
From test, its CO2Infiltration coefficient is 1420barrer, CO2/CH4Separation factor is 29；It is used for separating CO by this hybridized film2Volume
Mark is the CO of 10%2/N2Mixed gas separation is tested, its CO2Infiltration coefficient is 1561barrer, CO2/N2Separation factor is 79.
Embodiment 4: prepare chitosan-modified mesoporous silicon oxide and fill hybridized film.
The thickness of this hybridized film is 105 μm, by the polyoxyethylene that 12.5g mass fraction is 4%-polycaprolactam block altogether
The functionalization hollow Nano hydrogel composition of polymers and 0.1g, in described polyoxyethylene-polycaprolactam block copolymer, polyoxy
Ethylene segment accounts for the 60% of block copolymer mass fraction, and polycaprolactam segment accounts for the 40% of block copolymer mass fraction,
Its preparation method the difference is that only with above-described embodiment 1: in step 3, by chitosan-modified mesoporous silicon oxide consumption
Become 0.1g from 0.025g, finally give the chitosan-modified mesoporous silicon oxide that thickness is 105 μm homogenizing and fill hybridized film.Figure
4 is the SEM sectional drawing of the hybridized film that embodiment 4 prepares.
Under the conditions of room temperature, 1bar, it is used for separating CO by this hybridized film2Volume fraction is the CO of 30%2/CH4Mixing edema caused by disorder of QI
From test, its CO2Infiltration coefficient is 1835barrer, CO2/CH4Separation factor is 36；It is used for separating CO by this hybridized film2Volume
Mark is the CO of 10%2/N2Mixed gas separation is tested, its CO2Infiltration coefficient is 1943barrer, CO2/N2Separation factor is 85.
Comparative example: preparation is filled without chitosan-modified mesoporous silicon oxide1657 pure films.
The thickness of this film is 70 μm.Its preparation method is: weigh 0.5g polyoxyethylene-polycaprolactam block copolymer
(trade name1657), 3.6g deionized water and 8.4g dehydrated alcohol add in container, be placed in the water bath with thermostatic control of 80 DEG C
In, reflux under 500r/min stirring 2h, makes block copolymer all dissolve, is then cooled to room temperature standby.By above-mentioned macromolecule
Solution is poured in the glass plate of cleaning, is dried more than 24h under room temperature, then 45 DEG C, be dried 24h under vacuum condition, obtain
Thickness is 70 μm1657 pure films, Fig. 5 is the SEM sectional drawing of this film.
Under the conditions of room temperature, 1bar, it is used for separating CO by this hybridized film2Volume fraction is the CO of 30%2/CH4Mixing edema caused by disorder of QI
From test, its CO2Infiltration coefficient is 450barrer, CO2/CH4Separation factor is 15；It is used for separating CO by this hybridized film2Volume
Mark is the CO of 10%2/N2Mixed gas separation is tested, its CO2Infiltration coefficient is 460barrer, CO2/N2Separation factor is 49.
To sum up, prepared chitosan-modified mesoporous silicon oxide can be drawn according to above-described embodiment 1-4 and comparative example
Fill hybridized film and there is high osmosis and high separation factor, be primarily due to chitosan-modified mesoporous silicon oxide and improve high score
The compatibility between subbase matter and inorganic particulate, improve CO2Vector contg and add the water content in film.Compared to without shell
Polysaccharide modifies what mesoporous silicon oxide was filled1657 pure films, chitosan-modified mesoporous silicon oxide is filled hybridized film and is existed
CO2/CH4CO in gaseous mixture2Flux improves 4 times, CO2/CH4Separation factor improves 2.4 times；At CO2/N2CO in gaseous mixture2Logical
Amount improves 4.2 times, CO2/N2Separation factor improves 1.73 times.
Although above in conjunction with accompanying drawing, invention has been described, but the invention is not limited in above-mentioned being embodied as
Mode, above-mentioned detailed description of the invention is only schematic rather than restrictive, and those of ordinary skill in the art is at this
Under the enlightenment of invention, without deviating from the spirit of the invention, it is also possible to make many variations, these belong to the present invention's
Within protection.
Claims (4)
1. a chitosan-modified mesoporous silicon oxide fills hybridized film, it is characterised in that: this hybridized film thickness 70-105 μm, and
By the polyoxyethylene that mass fraction is 60-98%-polycaprolactam block copolymer and chitosan-modified mesoporous silicon oxide group
Becoming, in described polyoxyethylene-polycaprolactam block copolymer, polyoxyethylene segment accounts for the 55-of block copolymer mass fraction
60%, polycaprolactam segment accounts for the 40-45% of block copolymer mass fraction.
The most chitosan-modified mesoporous silicon oxide fills the preparation method of hybridized film, it is characterised in that:
Comprise the following steps:
Step 1, the preparation of chitosan-modified mesoporous silicon oxide:
Step 1-1, to add mass concentration in a container be the cetyl trimethylammonium bromide solution of 0.002g/mL, then
It is added dropwise over the sodium hydroxide solution of 2.0mol/L so that the concentration of sodium hydroxide is 0.014mol/L, treats that oil bath reaches 80 DEG C
Continuing stirring 40min, be slowly added dropwise tetraethyl orthosilicate, tetraethyl orthosilicate is 1.43 times of added sodium hydroxide volume, keeps 80
Stopped reaction after 3h is reacted under the conditions of DEG C；Gained solution is carried out sucking filtration, is first washed with deionized 3 times, then washes with ethanol
Wash 1 time and obtain solid product；Gained solid product is put in cuvette, the vacuum drying oven of 40 DEG C is dried 48h, obtains
Mesoporous silicon oxide with template；
Step 1-2, the mesoporous silicon oxide of the band template weighing step 1-1 gained add in a container, are subsequently adding concentrated hydrochloric acid
With the volume ratio of methanol, concentrated hydrochloric acid and methanol is 1: 0.06, the meso-porous titanium dioxide silicon concentration obtaining band template is 0.009mg/mL
Solution, at temperature 65 DEG C condensing reflux stirring 48h；It is centrifuged gained solution afterwards separating, washes 3 times, anhydrous second
Alcohol is washed 1 time, after putting into the dry 48h of vacuum drying oven, obtains mesoporous silicon oxide；
Step 1-3, weigh a certain amount of chitosan, this chitosan is dissolved in the glacial acetic acid solution that mass fraction is 5%, room temperature
Mechanical agitation 24h, it is thus achieved that mass fraction is the chitosan solution of 1%；Weigh the mesoporous silicon oxide of step 1-2 gained, should
Meso-porous titanium dioxide Si powder is dispersed in ethanol solution, obtains the mesoporous silicon oxide mixture that mass fraction is 1%, ultrasonic
15min, and with the glacial acetic acid of pH=4.8 by described mesoporous silicon oxide mixture regulation to pH be 3.5-4.5；Add the most rapidly
Entering the γ-glycidyl ether oxygen propyl trimethoxy silicane with the quality such as mesoporous silicon oxide and form mixture A, room temperature continues to stir
Mix 3h；The chitosan solution that volume ratio is 2 times of mesoporous silicon oxide mixture is added in mixture A, 24h is stirred at room temperature, from
Edema with the heart involved is washed 3 times, washing with alcohol 1 time, after putting into the dry 48h of vacuum drying oven, it is thus achieved that chitosan-modified mesoporous silicon oxide；
The preparation of step 2, polyoxyethylene-polycaprolactam block copolymer solution:
In mass ratio 1: (10-50), polyoxyethylene-polycaprolactam block copolymer is added mass fraction is 65-75%'s
In ethanol, at temperature 75-80 DEG C, it is heated at reflux more than 75 DEG C, stirs 0.5-4h, make polyoxyethylene-polycaprolactam block
Copolymer is completely dissolved, and obtaining mass fraction is 2-7% polyoxyethylene-polycaprolactam block copolymer solution；
The preparation of step 3, chitosan-modified mesoporous silicon oxide filling hybridized film:
In mass ratio 1: the ratio of (100-300), the chitosan-modified mesoporous silicon oxide of gained in step 1 is added step 2
In the polyoxyethylene-polycaprolactam block copolymer solution prepared, stir 5-10h at room temperature, the casting solution of gained is fallen
Clean glass plate is cast, dries at room temperature, be then placed in vacuum drying oven removing the solvent of residual, obtain chitosan
Modify mesoporous silicon oxide and fill hybridized film.
The most chitosan-modified mesoporous silicon oxide fills the application of hybridized film, this hybridized film is used for
Separate CO2/CH4Mixture, its CO2Flux is 450-1835barrer, CO2/CH4Separation factor is 15-36.
The most chitosan-modified mesoporous silicon oxide fills the application of hybridized film, this hybridized film is used for
Separate CO2/N2Mixture, CO2Flux is 460-1943barrer, CO2/N2Separation factor is 49-85.
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| CN106492646B (en) * | 2017-01-16 | 2019-05-17 | 北京工业大学 | A kind of preparation method for the preferential mesoporous silicon oxide hybridized film of alcohol infiltration evaporation thoroughly |
| CN110339726B (en) * | 2019-07-10 | 2021-09-07 | 浙江海印数码科技有限公司 | Polystyrene microsphere/carbon nanotube composite modified hybrid polyethersulfone nanofiltration membrane as well as preparation method and application thereof |
| CN112007426B (en) * | 2020-07-08 | 2022-06-14 | 山东联科科技股份有限公司 | Preparation method of high-performance mesoporous silica-chitosan composite antibacterial filter sheet |
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