CN108993176A - Block polyetheramides-amination graphene oxide hydridization film preparation and its application - Google Patents
Block polyetheramides-amination graphene oxide hydridization film preparation and its application Download PDFInfo
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- CN108993176A CN108993176A CN201810855141.XA CN201810855141A CN108993176A CN 108993176 A CN108993176 A CN 108993176A CN 201810855141 A CN201810855141 A CN 201810855141A CN 108993176 A CN108993176 A CN 108993176A
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- 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
- B01D71/02—Inorganic material
- B01D71/021—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
- B01D53/228—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion characterised by specific membranes
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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
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- 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
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- 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
- B01D71/56—Polyamides, e.g. polyester-amides
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
Abstract
The invention discloses a kind of block polyetheramides-amination graphene oxide hybridized film, the hybridized film is made of block polyetheramides and amination graphene oxide.Its preparation process includes: to be reacted with the graphene oxide of Hummer method synthesis with 3- aminopropyl triethoxysilane, obtains amination graphene oxide.Amination graphene oxide and solution blending obtain casting solution, and the hybridized film is made through the tape casting.The raw material of hybridized film of the present invention is easy to get, and preparation process is easy to be controllable, and Pebax- amination graphene oxide hybridized film obtained is applied to CO2/CH4And CO2/N2Gas separation, CO2The relatively pure film of permeability improves 60%~100%, for CO2/CH4Separation, the relatively pure film of selectivity improves 30%~50%, for CO2/N2Separation, the relatively pure film of selectivity improves 10%~30%.Young's modulus promotes 2~4 times to former film simultaneously, and breaking strength promotes 2~3 times to former film.
Description
Technical field
The present invention relates to a kind of block polyetheramides-amination graphene oxide hydridization film preparation and its applications, belong to gas
Body seperation film field.
Background technique
Energy and environment problem is the critical issue of global common concern.In recent years, with CO in atmosphere2The increasing of concentration
Add, resulting " greenhouse effects " lead to global warming, glacial ablation, the deterioration of the ecological environment, cause extensive society and close
Note.
Traditional CO2Isolation technics has very much, and membrane separation process is a kind of emerging CO2Isolation technics has many unique
Advantage has very high development prospect.Hybrid organic-inorganic film is one kind of seperation film, combine polymer film toughness and
Inoranic membrane it is highly selective and heat-resist the advantages that.Currently used filler mainly has zeolite, molecular sieve, silicon nanoparticle
Son, titanium dioxide nano-particle etc..But inorganic particulate is compatible with the interface of polymer matrix after introducing inorganic particulate in film
Property is the greatest problem faced.And the interface compatibility of film and inorganic particulate can not only be improved after being modified inorganic particulate,
Improve boundary defect, moreover it is possible to improve permeability of the membrane and selection performance separating property.
Graphene has obtained very extensive research and application as a kind of novel filler in recent years, be it is a kind of very
There is the inorganic filling material of application prospect.Compared with existing inorganic material, graphene have unique structure, large specific surface area,
The features such as easy functional modification, mechanical property is good.The present invention aoxidizes the modified amination of 3- aminopropyl triethoxysilane
Graphene is mixed into block polyetheramides matrix, is prepared for a kind of block polyetheramides-amination graphene oxide hybridized film, has
The interface compatibility between graphene oxide and block polyetheramides is improved to effect, the gas point of film is simultaneously effective improved
From performance.
Summary of the invention
The present invention provides a kind of block polyetheramides-amination graphene oxide hybridized films.Preparation provided by the invention
Method process is simple to operation, environmentally protective, and prepared hybridized film can be applied to CO2Separation has good separation effect
Fruit.
Block polyetheramides prepared by the present invention-amination graphene oxide hybridized film is with a thickness of 40~100 microns.
It is 0.01%~30% that amination graphene oxide, which accounts for the mass fraction of hybridized film, in the hybridized film.
Block polyetheramides of the present invention-amination graphene oxide hybridized film preparation method, including following procedure:
Step 1 will use the graphene oxide ultrasonic disperse of Hummer method preparation in 3- aminopropyl triethoxysilane,
Dicyclohexylcarbodiimide is added as catalysts, is heated to and stirs certain time, it is then dry with ethyl alcohol centrifuge washing
It is dry, finally obtain the alcohol dispersion liquid of amination graphene oxide.
Block polyetheramides are added in the mixed liquor of water and ethyl alcohol by step 2, are heated and are stirred to dissolution, then plus
Enter a certain amount of amination graphene oxide dispersion, stirs and ultrasound, amination graphene oxide account for block polyetheramides
Mass fraction is 0%~30%.
The casting solution that block polyetheramides and amination graphene oxide that step 2 obtains are blended is poured on mold by step 3
In, block polyetheramides-amination graphene oxide hybridized film is obtained after dry.
Compared with the prior art, the advantages of the present invention are as follows: preparation process is easy to be controllable, and raw material is easy to get, mild condition, system
Block polyetheramides-amination graphene oxide the hybridized film obtained is applied to CO2/CH4Separation, the relatively pure film of selectivity promotes
30%~50%, CO2The relatively pure film of permeability improves 60%~100%；Applied to CO2/N2Separation, selectivity is opposite
Pure film improves 10%~30%, CO2The relatively pure film of permeability improves 60%~100%.Mechanical performance also has very big simultaneously
It is promoted, block polyetheramides of the present invention-amination graphene oxide hybridized film, when the mass fraction of amination graphene oxide is
When 0.1%~1%, the Young's modulus of hybridized film promotes 2~4 times to former film, and breaking strength promotes 2~3 times to former film.
Detailed description of the invention
Fig. 1 is the figure of block polyetheramides-amination graphene oxide hybridized film surface part SEM made from embodiment 3.
Specific embodiment
Detailed content of the invention is told about by the following examples, and providing embodiment is the convenience for understanding, definitely not
The limitation present invention.
Comparative example 1: pure block polyetheramides homogeneous membrane is prepared
It weighs 0.9g block polyetheramides (block polyetheramides that this comparative example is selected are pebax 1657) and is added to 22g
In the mixture of water and ethyl alcohol, the mass ratio of water and ethyl alcohol is that stirring 2h is all dissolved to macromolecule at 3: 7,80 DEG C, is obtained
Pebax1657 solution pours into clean Teflon mould after standing and defoaming, at room temperature it is dry for 24 hours, it is then true at 45 DEG C
Drying for 24 hours, obtains thick about 70 μm of homogeneous membrane, which is pure block polyetheramides (Pebax) homogeneous membrane in empty baking oven；
The film is subjected to pure CO under the conditions of 35 DEG C, 2bar2, pure CH4, pure N2Permeance property test, CO2Infiltration coefficient is
96.4barrer (1barrer=10-10cm3(STP)cm/(cm2S cmHg)), CO2/CH4And CO2/N2Selectively it is respectively
12.29 with 39.18.Effective length 1cm is made in the film, the Rectangular samples of width 0.5cm carry out tensile strength test, in room
Temperature, tensile speed test film under conditions of being 5mm/min, and measuring Young's modulus is 46.26Mpa, and breaking strength is
7.16Mpa。
Embodiment 1:
Block polyetheramides-amination graphene oxide hybridized film is by block polyetheramides and amination graphene oxide structure
At film thickness is 72 μm, wherein the mass percent that amination graphene oxide accounts for block polyetheramides is 0.3%.
Above-mentioned block polyetheramides-amination graphene oxide hybridized film the preparation method is as follows:
Graphene oxide is prepared using Hummers, the concentrated sulfuric acid (150mL) that mass fraction is 98% is placed on 250mL
In round-bottomed flask, stirred in ice-water bath.Natural graphite powder (2.0g) and NaNO are added in whipping process3(1.0g).Then
In batches by KMnO4(7.0g) is added in mixture in 30min.Mixed solution is maintained at 0-5 DEG C and persistently stirs 1h；It is mixed
It closes object to move on in water bath with thermostatic control, temperature is raised to 55 DEG C of stirring 4h；It is slowly added to 150mL ice deionized water into mixture, adds
The temperature that cannot make mixture during adding is more than 100 DEG C, and mixture is allowed to continue to stir 30min at 97 DEG C；It will be in reactant
It pours into 50mL to go to dilute from water, 30% hydrogen peroxide 50ml is then added, removes wherein remaining potassium permanganate and manganese dioxide.
It filters, is sufficiently washed with the hydrochloric acid that mass fraction is 5% while hot, be washed with distilled water to pH then as neutrality, obtain graphite oxide
Alkene.
The graphene oxide powder (GO) of the above-mentioned preparation of 100mg and 50mg dicyclohexylcarbodiimide (DCC) powder are added
Enter into 100mL 3- aminopropyl triethoxysilane (APTS), ultrasound 2h after mixing.Then under the conditions of 70 DEG C of oil bath heatings
Stirring is for 24 hours.It is used dehydrated alcohol eccentric cleaning 3 times after the completion of heating stirring, and is made into the graphene oxide ethyl alcohol of 2mg/ml concentration
Dispersion liquid.
It weighs 0.9g block polyetheramides (block polyetheramides that the present embodiment is selected are pebax 1657) and is added to 22g
In the mixture of water and ethyl alcohol, the mass ratio of water and ethyl alcohol is that stirring 2h is all dissolved to macromolecule at 3: 7,80 DEG C, is obtained
Pebax1657 solution；It is molten that the amination graphene oxide dispersion obtained above of 1.35ml is added to above-mentioned Pebax1657
In liquid, magnetic agitation 4h, ultrasonic 1h are poured into clean Teflon mould after standing and defoaming, at room temperature it is dry for 24 hours, with
Drying for 24 hours, obtains thick about 72 μm of homogeneous membrane, which is block polyetheramides in 45 DEG C of vacuum drying ovens afterwards
(Pebax)-amination graphene oxide hybridized film.
The block polyetheramides that embodiment 1 is prepared-amination graphene oxide hybridized film is in 35 DEG C, 2bar condition
It is lower to carry out pure CO2, pure CH4, pure N2Permeance property test, CO2Infiltration coefficient is 158barrer (1barrer=10-10cm3(STP)
cm/(cm2S cmHg)), CO2/CH4And CO2/N2Selectivity is respectively 13.17 and 43.89.Effective length 1cm is made in the film,
The Rectangular samples of width 0.5cm carry out tensile strength test, under conditions of room temperature, tensile speed are 5mm/min to film into
Row test, measuring Young's modulus is 100.67Mpa, breaking strength 11.95Mpa.
Embodiment 2:
Block polyetheramides-amination graphene oxide hybridized film is by block polyetheramides and amination graphene oxide structure
At film thickness is 79 μm, wherein the mass percent that amination graphene oxide accounts for block polyetheramides is 0.5%.
Above-mentioned block polyetheramides-amination graphene oxide hybridized film the preparation method is as follows:
Amination graphene oxide dispersion is prepared using method same as Example 1.
It weighs 0.9g block polyetheramides (block polyetheramides that the present embodiment is selected are pebax 1657) and is added to 22g
In the mixture of water and ethyl alcohol, the mass ratio of water and ethyl alcohol is that stirring 2h is all dissolved to macromolecule at 3: 7,80 DEG C, is obtained
Pebax1657 solution；It is molten that the amination graphene oxide dispersion obtained above of 2.25ml is added to above-mentioned Pebax1657
In liquid, magnetic agitation 4h, ultrasonic 1h are poured into clean Teflon mould after standing and defoaming, at room temperature it is dry for 24 hours, with
Drying for 24 hours, obtains thick about 79 μm of homogeneous membrane, which is block polyetheramides-amino in 45 DEG C of vacuum drying ovens afterwards
Change graphene oxide hybridized film.
The block polyetheramides that embodiment 2 is prepared-amination graphene oxide hybridized film is in 35 DEG C, 2bar condition
It is lower to carry out pure CO2, pure CH4, pure N2Permeance property test, CO2Infiltration coefficient is 174barrer (1barrer=10-10cm3(STP)
cm/(cm2S cmHg)), CO2/CH4And CO2/N2Selectivity is respectively 13.38 and 43.5.Effective length 1cm is made in the film, it is wide
The Rectangular samples for spending 0.5cm carry out tensile strength test, carry out under conditions of room temperature, tensile speed are 5mm/min to film
Test, measuring Young's modulus is 108.55Mpa, breaking strength 13.35Mpa.
Embodiment 3:
Block polyetheramides-amination graphene oxide hybridized film is by block polyetheramides and amination graphene oxide structure
At film thickness is 89 μm, wherein the mass percent that amination graphene oxide accounts for block polyetheramides is 0.7%.
Above-mentioned block polyetheramides-amination graphene oxide hybridized film the preparation method is as follows:
Amination graphene oxide dispersion is prepared using method same as Example 1.
It weighs 0.9g block polyetheramides (block polyetheramides that the present embodiment is selected are pebax 1657) and is added to 22g
In the mixture of water and ethyl alcohol, the mass ratio of water and ethyl alcohol is that stirring 2h is all dissolved to macromolecule at 3: 7,80 DEG C, is obtained
Pebax1657 solution；It is molten that the amination graphene oxide dispersion obtained above of 3.15ml is added to above-mentioned Pebax1657
In liquid, magnetic agitation 4h, ultrasonic 1h are poured into clean Teflon mould after standing and defoaming, at room temperature it is dry for 24 hours, with
Drying for 24 hours, obtains thick about 89 μm of homogeneous membrane, which is block polyetheramides-amino in 45 DEG C of vacuum drying ovens afterwards
Change graphene oxide hybridized film.
The block polyetheramides that embodiment 3 is prepared-amination graphene oxide hybridized film is in 35 DEG C, 2bar condition
It is lower to carry out pure CO2, pure CH4, pure N2Permeance property test, CO2Infiltration coefficient is 172barrer (1barrer=10-10cm3(STP)
cm/(cm2S cmHg)), CO2/CH4And CO2/N2Selectivity is respectively 17.20 and 45.20.Effective length 1cm is made in the film,
The Rectangular samples of width 0.5cm carry out tensile strength test, under conditions of room temperature, tensile speed are 5mm/min to film into
Row test, measuring Young's modulus is 125.96Mpa, breaking strength 14.75Mpa.
Comparative example 2: block polyetheramides-graphene oxide hybridized film is prepared
Graphene oxide is prepared using method identical with comparative example 2.
The graphene oxide powder for taking 100mg above-mentioned is added in the pure water of 50ml, ultrasonic disperse 2h, and obtaining concentration is 2mg/
The graphene oxide dispersion of ml.
It weighs 0.9g block polyetheramides (block polyetheramides that this comparative example is selected are pebax 1657) and is added to 22g
In the mixture of water and ethyl alcohol, the mass ratio of water and ethyl alcohol is that stirring 2h is all dissolved to macromolecule at 3: 7,80 DEG C, is obtained
Pebax1657 solution；The graphene oxide dispersion obtained above of 3.15ml is added in above-mentioned Pebax1657 solution,
Magnetic agitation 4h, ultrasonic 1h are poured into clean Teflon mould after standing and defoaming, at room temperature it is dry for 24 hours, then 45
In DEG C vacuum drying oven it is dry for 24 hours, obtain thick about 84 μm of homogeneous membrane, which is block polyetheramides-graphene oxide
Hybridized film.
Block polyetheramides-graphene oxide hybridized film that comparative example 4 is prepared is carried out under the conditions of 35 DEG C, 2bar
Pure CO2, pure CH4, pure N2Permeance property test, CO2Infiltration coefficient is 111barrer (1barrer=10-10cm3(STP)cm/
(cm2S cmHg)), CO2/CH4And CO2/N2Selectivity is respectively 12.88 and 41.23.Effective length 1cm, width is made in the film
The Rectangular samples of 0.5cm carry out tensile strength test, survey under conditions of room temperature, tensile speed are 5mm/min to film
Examination, measuring Young's modulus is 40.18Mpa, breaking strength 6.48Mpa.
Embodiment 4:
Block polyetheramides-amination graphene oxide hybridized film is by block polyetheramides and amination graphene oxide structure
At film thickness is 76 μm, wherein the mass percent that amination graphene oxide accounts for block polyetheramides is 0.9%.
Above-mentioned block polyetheramides-amination graphene oxide hybridized film the preparation method is as follows:
Amination graphene oxide dispersion is prepared using method same as Example 1.
It weighs 0.9g block polyetheramides (block polyetheramides that the present embodiment is selected are pebax 1657) and is added to 22g
In the mixture of water and ethyl alcohol, the mass ratio of water and ethyl alcohol is that stirring 2h is all dissolved to macromolecule at 3: 7,80 DEG C, is obtained
Pebax1657 solution；It is molten that the amination graphene oxide dispersion obtained above of 4.05ml is added to above-mentioned Pebax1657
In liquid, magnetic agitation 4h, ultrasonic 1h are poured into clean Teflon mould after standing and defoaming, at room temperature it is dry for 24 hours, with
Drying for 24 hours, obtains thick about 76 μm of homogeneous membrane, which is block polyetheramides-amino in 45 DEG C of vacuum drying ovens afterwards
Change graphene oxide hybridized film.
The block polyetheramides that embodiment 4 is prepared-amination graphene oxide hybridized film is in 35 DEG C, 2bar condition
It is lower to carry out pure CO2, pure CH4, pure N2Permeance property test, CO2Infiltration coefficient is 152barrer (1barrer=10-10cm3(STP)
cm/(cm2S cmHg)), CO2/CH4And CO2/N2Selectivity is respectively 13.81 and 43.3.Effective length 1cm is made in the film, it is wide
The Rectangular samples for spending 0.5cm carry out tensile strength test, carry out under conditions of room temperature, tensile speed are 5mm/min to film
Test, measuring Young's modulus is 93.96Mpa, breaking strength 13.03Mpa.
Fig. 1 is the figure of block polyetheramides-amination graphene oxide hybridized film surface part SEM made from embodiment 3.
It can be clearly seen that the amination graphene oxide of introducing from figure, and distribute very evenly, illustrate that the amination aoxidizes
Graphene has good interface compatibility, is conducive to the promotion of gas separating property, shows the successful preparation of hybridized film.It is logical
Comparative example and the gas separating property comparative illustration of embodiment are crossed in the identical situation of doping, amination graphene oxide
There is better gas permeability and separating property with the hybridized film of block polyetheramides.
Although the invention is not limited to above-mentioned specific embodiment party above in conjunction with figure to the present invention just description
Formula, the above mentioned embodiment is only schematical, rather than restrictive, and the platform technology personnel of this field are in this hair
Under bright enlightenment, without deviating from the spirit of the invention, many variations can also be made, these belong to guarantor of the invention
Within shield.
Claims (6)
1. a kind of block polyetheramides-amination graphene oxide hybridized film, it is characterised in that: the block polyetheramides-amino
Change graphene oxide hybridized film be made of block polyetheramides and amination graphene oxide, wherein amination graphite oxide by
Graphene oxide and 3- aminopropyl triethoxysilane react generation under catalytic condition.
2. a kind of block polyetheramides as described in claim 1-amination graphene oxide hybridized film, it is characterised in that this is miscellaneous
Change film with a thickness of 40~100 microns.
3. a kind of block polyetheramides as described in claim 1-amination graphene oxide hybridized film, it is characterised in that this is miscellaneous
Changing amination graphene oxide in film to account for the mass fraction of hybridized film is 0.01%~30%.
4. a kind of block polyetheramides as described in claim 1-amination graphene oxide hybridized film preparation method, including
Following procedure:
Step 1 in 3- aminopropyl triethoxysilane, will be added using the graphene oxide ultrasonic disperse of Hummer method preparation
Dicyclohexylcarbodiimide is heated to and stirs certain time as catalysts, then dry with ethyl alcohol centrifuge washing, most
The alcohol dispersion liquid of amination graphene oxide is obtained afterwards.
Block polyetheramides are added in the mixed liquor of water and ethyl alcohol by step 2, are heated and are stirred to dissolution, are then added one
Quantitative amination graphene oxide dispersion, is stirred and ultrasound, amination graphene oxide account for the quality of block polyetheramides
Score is 0%~30%.
The casting solution that step 3, the block polyetheramides that step 2 is obtained and amination graphene oxide are blended in a mold,
Block polyetheramides-amination graphene oxide hybridized film is obtained after drying.
5. a kind of block polyetheramides as described in claim 1-amination graphene oxide hybridized film are applied to CO2/CH4's
Separation, the relatively pure film of selectivity improve 30%~50%, CO2The relatively pure film of permeability improves 60%~100%；It is applied to
CO2/N2Separation, the relatively pure film of selectivity improves 10%~30%, CO2The relatively pure film of permeability improves 60%~
100%.
6. a kind of block polyetheramides as described in claim 1 (Pebax)-amination graphene oxide hybridized film, work as amino
When the mass fraction for changing graphene oxide is 0.1%~1%, the Young's modulus of hybridized film promotes 2~4 times to former film, fracture
2~3 times to former film of strength enhancing.
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| CN113881218A (en) * | 2021-10-18 | 2022-01-04 | 东莞市迪彩塑胶五金有限公司 | Antistatic agent for material forming and processing and preparation method thereof |
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Application publication date: 20181214 |