CN106975372A - The mixed substrate membrane containing nano-grade molecular sieve and preparation method and application filled based on flaky material - Google Patents
The mixed substrate membrane containing nano-grade molecular sieve and preparation method and application filled based on flaky material Download PDFInfo
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- CN106975372A CN106975372A CN201710252642.4A CN201710252642A CN106975372A CN 106975372 A CN106975372 A CN 106975372A CN 201710252642 A CN201710252642 A CN 201710252642A CN 106975372 A CN106975372 A CN 106975372A
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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
- B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
- B01D71/62—Polycondensates having nitrogen-containing heterocyclic rings in the main chain
- B01D71/64—Polyimides; Polyamide-imides; Polyester-imides; Polyamide acids or similar polyimide precursors
-
- 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
-
- 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
- B01D69/14—Dynamic membranes
- B01D69/141—Heterogeneous membranes, e.g. containing dispersed material; Mixed matrix membranes
- B01D69/148—Organic/inorganic mixed matrix membranes
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
- C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
- C10L3/10—Working-up natural gas or synthetic natural gas
- C10L3/101—Removal of contaminants
- C10L3/102—Removal of contaminants of acid contaminants
- C10L3/104—Carbon dioxide
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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 present invention discloses a kind of mixed substrate membrane containing nano-grade molecular sieve filled based on flaky material, and the nano silver slice that the mixed substrate membrane containing nano-grade molecular sieve is dispersed in polyether block polyamides copolymer body by polyether block polyamides copolymer and filling is constituted.The mixed substrate membrane containing nano-grade molecular sieve is to CO2/CH4Gaseous mixture and CO2/N2The Selective Separation CO of gaseous mixture2Result of the test shows, its permselective property data has exceeded the 2008Robeson upper limits, illustrate the carbon dioxide separation performance that effective carbon-dioxide transmission channels reinforced film is constructed using nano silver slice smooth surface, overcome that " trade off " effects, the gas permeability and selectivity for improving film, which are one, effective improves the method for mixed-matrix film properties.
Description
Technical field
The invention belongs to field of membrane material, and in particular to a kind of mixed substrate membrane containing nano-grade molecular sieve filled based on flaky material, particularly
The membrane material separated for carbon dioxide, and its preparation method and application.
Background technology
Natural gas and biogas are usually contained in important industrial chemicals and clean energy resource, freshly harvested natural gas and biogas
The sour gas such as carbon dioxide, these sour gas not only influence gaseous mass, and can heavy corrosion pipeline and equipment, institute
So that these sour gas must be being removed before, and carbon trapping turns into a necessary and crucial industrial process.It is efficiently low
Energy consumption and environment-friendly collecting carbonic anhydride technology are the keys for solving energy gas purifying problem.Membrane technology with its efficiently,
The features such as green, low-carbon, shows good development prospect, exploitation high osmosis, high selectivity two in collecting carbonic anhydride field
Carbonoxide separation membrane material has important theory value and realistic meaning.
Gas separation membrane material refers to the material to material with selective penetrated property, and organic high molecular layer is separated as gas
Membrane material has the characteristics that：With good film forming, heat endurance, mechanical performance and solvent resistant and other chemical substances.
However, it is nearly all it is ready-made, can all exist with the high polymer material of film forming one it is common the problem of：Every gas permeability coefficient
Big film, it is relatively low that it separates selection coefficient；The high film of every separation selection coefficient, its gas permeability coefficient is relatively low, i.e. " trade-
Off " effects.Mixed substrate membrane containing nano-grade molecular sieve can overcome a class membrane material of " trade-off " effect to turn into this area as one kind
Study hotspot.Currently used for the particle filled composite prepared used in composite membrane for example zeolite, carbon molecular sieve, nanotube, metal organic frame,
Graphene etc..
In recent years, with continuing to develop that researcher studies in terms of mixed substrate membrane containing nano-grade molecular sieve, carbon dioxide is constructed in film
Transmission channels thought efficiently separates the concern that method has caused researchers as a kind of.
The content of the invention
The technical problem to be solved in the present invention is to overcome existing defect to be used for carbon dioxide separation there is provided one kind
Based on flaky material fill mixed substrate membrane containing nano-grade molecular sieve.
In order to solve the above-mentioned technical problem, the invention provides following technical scheme：
Based on flaky material fill mixed substrate membrane containing nano-grade molecular sieve, the mixed substrate membrane containing nano-grade molecular sieve by polyether-polyamide block copolymer with
And filling is dispersed in the nano silver slice composition in polyether-polyamide block copolymer body.
Preferably, the mass ratio of the polyether-polyamide block copolymer and nano silver slice is 1:0.02~1:0.08.
It is highly preferred that the mass ratio of the polyether-polyamide block copolymer and nano silver slice is 1:0.04~1:0.06.
Preferably, the thickness of the mixed substrate membrane containing nano-grade molecular sieve is 50~80 μm.
The preparation method of above-mentioned mixed substrate membrane containing nano-grade molecular sieve, including：Polyether-polyamide block copolymer is first dissolved in alcohol-water
In the mixed solvent, adds nano silver slice, after mixing, is cast, is dried to obtain the mixed substrate membrane containing nano-grade molecular sieve.
Preferably, the nano silver slice is made by the method comprised the following steps：First by silver nitrate and polyvinyl pyrrole
Alkanone is added to the water, after dissolving, sequentially adds sodium citrate, sodium borohydride, hydrogen peroxide and hydrazine hydrate, after the completion of reaction, point
From obtaining nano silver slice.Add after sodium citrate, treat that solution is changed into light grey, add sodium borohydride, add after sodium borohydride
Hydrogen peroxide, stirring reaction (about 30min) are added immediately, then hydrazine hydrate is added dropwise, continues stirring reaction (about 1h), and shading is stood.Its
In, polyvinylpyrrolidone promotes to form uniform nanometer sheet as dispersant；Sodium citrate is controlled { 100 } as stabilizer
The speed of growth in face, promotes generation nanometer sheet；Sodium borohydride is risen as reducing agent, reduces silver ion；Hydrogen peroxide as oxidant,
The reduction of silver is reduced, irregular small silver particles are etched；Hydrazine hydrate makes the silver-colored simple substance newly reduced be put down along horizontal as reducing agent
Look unfamiliar length.
Preferably, the mass ratio of the silver nitrate, polyvinylpyrrolidone and sodium citrate is 1:0.5:(0.1~
0.09)；The silver nitrate, sodium borohydride, the mol ratio of hydrogen peroxide and hydrazine hydrate are 1:0.001:(4.5~5):(4~4.5),
Preferably, the mol ratio of the silver nitrate, sodium borohydride, hydrogen peroxide and hydrazine hydrate is 1:0.001:4.9:4.
Above-mentioned mixed substrate membrane containing nano-grade molecular sieve can be used for Selective Separation CO2Gas.As UF membrane removes the CO in natural gas or biogas2
Gas.
Pebax- nano silver slice mixed substrate membrane containing nano-grade molecular sieves are to CO2/CH4Gaseous mixture and CO2/N2The Selective Separation CO of gaseous mixture2Examination
Test result to show, its permselective property data has exceeded the 2008Robeson upper limits, illustrate to construct using nano silver slice smooth surface
The carbon dioxide separation performance of effective carbon-dioxide transmission channels reinforced film, overcomes " trade-off " effect, improves the gas of film
Permeability and selectivity are the methods of an effective improvement mixed-matrix film properties.
Brief description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, and constitutes a part for specification, the reality with the present invention
Applying example is used to explain the present invention together, is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is the scanning electron microscope (SEM) photograph of the nano silver slice obtained by embodiment 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of the Pebax- nano silver slice mixed substrate membrane containing nano-grade molecular sieve sections obtained by embodiment 1；
Fig. 3 is the scanning electron microscope (SEM) photograph of the Pebax- nano silver slice mixed substrate membrane containing nano-grade molecular sieve sections obtained by embodiment 2；
Fig. 4 is the scanning electron microscope (SEM) photograph of the Pebax- nano silver slice mixed substrate membrane containing nano-grade molecular sieve sections obtained by embodiment 3；
Fig. 5 is the scanning electron microscope (SEM) photograph of the Pebax- nano silver slice mixed substrate membrane containing nano-grade molecular sieve sections obtained by embodiment 4；
Fig. 6 is the scanning electron microscope (SEM) photograph of the pure Pebax films section obtained by comparative example.
Embodiment
The preferred embodiments of the present invention are illustrated below in conjunction with accompanying drawing, it will be appreciated that preferred reality described herein
Apply example to be merely to illustrate and explain the present invention, be not intended to limit the present invention.
Embodiment 1
Prepare Pebax- nano silver slice mixed substrate membrane containing nano-grade molecular sieves, the thickness of the mixed substrate membrane containing nano-grade molecular sieve is 55 μm, the mixed substrate membrane containing nano-grade molecular sieve with
Polyether-polyamide block copolymer (1657, it is abbreviated as Pebax) it is membrane matrix, nano silver slice is added in membrane matrix,
Wherein, the mass ratio 1 of Pebax and nano silver slice：0.02, the preparation process of the mixed substrate membrane containing nano-grade molecular sieve is as follows：
Step 1, nano silver slice are prepared using solution phase chemical reduction：
Take silver nitrate (AgNO3, 3.4g) and polyvinylpyrrolidone (PVP, 1.7g) be dissolved in deionized water (100mL),
Ultrasonic disperse, then pours into mechanical agitation in three-necked flask (600r/min) by solution, and 4mL sodium citrates are added into solution
(0.3mol/L), treats that solution is changed into light grey, 1mL sodium borohydrides (0.02mol/L) solution is added into solution, and be added immediately
10mL hydrogen peroxide (30%), continues to stir 30min.5mL hydrazine hydrates (80%) are dissolved in 50mL deionized waters, dripped by constant pressure
Liquid funnel is slowly added into reaction solution, after dripping off, and adjusts rotating speed 800r/min, continues to stir 1h.Reaction solution is poured into totally
Beaker in, at 25 DEG C seal shading place 48h, centrifugation (8000r/min) washing, dry after obtain gray precipitate, produce
Nano silver slice.Fig. 1 is the scanning electron microscope (SEM) photograph of the nano silver slice obtained by embodiment 1.
Step 2, weigh 2.5g Pebax grain dissolutions concentration for 70wt% ethanol water in, 80 DEG C stirring
8h so that Pebax particles all dissolve, prepares mass fraction for 4%Pebax solution, standby.
Step 3, nano silver slice made from step 1 (0.05g) is added in Pebax solution made from step 2, in room temperature
Lower stirring 8h, obtains casting solution.The casting solution of gained is poured on the ultra-flat surface ware of cleaning and is cast, 48h is dried at 25 DEG C,
Then put it into 50 DEG C of vacuum drying ovens and remove the solvent of residual, obtain Pebax- nano silver slice mixed substrate membrane containing nano-grade molecular sieves, obtain thickness
Spend the mixed substrate membrane containing nano-grade molecular sieve for 55 μm.Fig. 2 is the scanning electron microscope (SEM) photograph of obtained Pebax- nano silver slice mixed substrate membrane containing nano-grade molecular sieve sections.
Under the conditions of 25 DEG C, 2bar, Pebax- nano silver slices mixed substrate membrane containing nano-grade molecular sieve is used to separate CO2Volume fraction is 10%
CO2/CH4Gaseous mixture, its CO2Flux is 340barrer, CO2/CH4Selectivity is 31；The mixed substrate membrane containing nano-grade molecular sieve is used for CO2Body
Fraction is 10% CO2/N2Gaseous mixture, its CO2Flux is 316barrer, CO2/N2Selectivity 55.
Embodiment 2
As different from Example 1：The thickness of mixed substrate membrane containing nano-grade molecular sieve is 64 μm, wherein, the mass ratio of Pebax and nano silver slice
1：0.04.Fig. 3 is the scanning electron microscope (SEM) photograph of obtained Pebax- nano silver slice mixed substrate membrane containing nano-grade molecular sieve sections.
Under the conditions of 25 DEG C, 2bar, obtained Pebax- nano silver slices mixed substrate membrane containing nano-grade molecular sieve is used to separate CO2Volume integral
Number is 10% CO2/CH4Gaseous mixture, its CO2Flux is 443barrer, CO2/CH4Selectivity is 40；The mixed substrate membrane containing nano-grade molecular sieve is used
In separation CO2Volume fraction is 10% CO2/N2Gaseous mixture, its CO2Flux is 404barrer, CO2/N2Selectivity 58.
Embodiment 3
With embodiment 1 except that：The thickness of film is 76 μm, wherein, the mass ratio 1 of Pebax and nano silver slice：
0.06.Fig. 4 is the scanning electron microscope (SEM) photograph of obtained Pebax- nano silver slice mixed substrate membrane containing nano-grade molecular sieve sections.
Under the conditions of 25 DEG C, 2bar, obtained Pebax- nano silver slices mixed substrate membrane containing nano-grade molecular sieve is used to separate CO2Volume integral
Number is 10% CO2/CH4Gaseous mixture, its CO2Flux is 349barrer, CO2/CH4Selectivity is 44；The mixed substrate membrane containing nano-grade molecular sieve is used
In separation CO2Volume fraction is 10% CO2/N2Gaseous mixture, its CO2Flux is 365barrer, CO2/N2Selectivity 56.
Embodiment 4
With embodiment 1 except that：The thickness of film is 79 μm, wherein, the mass ratio 1 of Pebax and nano silver slice：
0.08.Fig. 5 is the scanning electron microscope (SEM) photograph of obtained Pebax- nano silver slice mixed substrate membrane containing nano-grade molecular sieve sections.
Under the conditions of 25 DEG C, 2bar, obtained Pebax- nano silver slices mixed substrate membrane containing nano-grade molecular sieve is used to separate CO2Volume integral
Number is 10% CO2/CH4Gaseous mixture, its CO2Flux is 221barrer, CO2/CH4Selectivity is 31.7；By the mixed substrate membrane containing nano-grade molecular sieve
For separating CO2Volume fraction is 10% CO2/N2Gaseous mixture, its CO2Flux is 226barrer, CO2/N2Selectivity 41.5.
Comparative example 1
2.5g Pebax grain dissolutions are weighed in the ethanol water that concentration is 70wt%, after 80 DEG C are stirred 8h, are obtained
To casting solution.The casting solution of gained is poured on the ultra-flat surface ware of cleaning and is cast, 48h is dried at room temperature for, is then put
Enter 24h in 50 DEG C of vacuum drying ovens and, to remove the solvent of residual, obtain the Pebax films that thickness is 60 μm.Fig. 6 is obtained pure
The scanning electron microscope (SEM) photograph of Pebax film sections.
Under the conditions of 25 DEG C, 2bar, obtained pure Pebax films are used to separate CO2Volume fraction is 10% CO2/
CH4Gaseous mixture, its CO2Flux is 281barrer, CO2/CH4Selectivity is 30；For separating CO2Volume fraction is 10%
CO2/N2Gaseous mixture, its CO2Flux is 305barrer, CO2/N2Selectivity 54.
Comparative example 2
Pebax- nano-Ag particles mixed substrate membrane containing nano-grade molecular sieves are prepared, the thickness of the mixed substrate membrane containing nano-grade molecular sieve is 76 μm, the mixed substrate membrane containing nano-grade molecular sieve
Using Pebax as membrane matrix, nano-Ag particles are added in membrane matrix, wherein, the mass ratio 1 of Pebax and nano-Ag particles：
0.06, the preparation process of the mixed substrate membrane containing nano-grade molecular sieve is as follows：
Step 1, nano-Ag particles are prepared using hydro-thermal method：
Take cetyl trimethylammonium bromide (CTAB, 1.0g) to be dissolved in deionized water (20mL), after stirring and dissolving, add
The solution dissolved is poured into reactor and is built in 150 DEG C by 0.25mol/L glucose solution 10mL, further stirring and dissolving
Muffle reaction in furnace 8h, after the completion of reaction, by solution centrifugal wash dry after, obtain nano-Ag particles product.
Step 2, weigh 2.5g Pebax grain dissolutions concentration for 70wt% ethanol water in, 80 DEG C stirring
8h so that Pebax particles all dissolve, prepares mass fraction for 4%Pebax solution, standby.
Step 3, nano-Ag particles made from step 1 (0.15g) are added in Pebax solution made from step 2, in room
The lower stirring 8h of temperature, obtains casting solution.The casting solution of gained is poured on the ultra-flat surface ware of cleaning and is cast, is dried at 25 DEG C
48h, then puts it into 50 DEG C of vacuum drying ovens and removes the solvent of residual, obtain Pebax- nano-Ag particles mixed substrate membrane containing nano-grade molecular sieves,
Obtain the mixed substrate membrane containing nano-grade molecular sieve that thickness is 76 μm.
Under the conditions of 25 DEG C, 2bar, Pebax- nano-Ag particles mixed substrate membrane containing nano-grade molecular sieve is used to separate CO2Volume fraction is
10% CO2/CH4Gaseous mixture, its CO2Flux is 304barrer, CO2/CH4Selectivity is 30；The mixed substrate membrane containing nano-grade molecular sieve is used for
CO2Volume fraction is 10% CO2/N2Gaseous mixture, its CO2Flux is 319barrer, CO2/N2Selectivity 54.
Table 1 is Pebax- Nano Silver mixed substrate membrane containing nano-grade molecular sieve Selective Separations CO2Result
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still may be used
To be modified to the technical scheme described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic.
Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., should be included in the present invention's
Within protection domain.
Claims (9)
1. the mixed substrate membrane containing nano-grade molecular sieve filled based on flaky material, the mixed substrate membrane containing nano-grade molecular sieve by polyether-polyamide block copolymer and
Filling is dispersed in the nano silver slice composition in polyether-polyamide block copolymer body.
2. mixed substrate membrane containing nano-grade molecular sieve according to claim 1, it is characterised in that：The polyether-polyamide block copolymer is with receiving
The mass ratio of rice silver strip is 1:0.02~1:0.08.
3. mixed substrate membrane containing nano-grade molecular sieve according to claim 2, it is characterised in that：The polyether-polyamide block copolymer is with receiving
The mass ratio of rice silver strip is 1:0.04~1:0.06.
4. mixed substrate membrane containing nano-grade molecular sieve according to claim 1, it is characterised in that：The thickness of the mixed substrate membrane containing nano-grade molecular sieve is 50~80 μ
m。
5. the preparation method of any mixed substrate membrane containing nano-grade molecular sieves of claim 1-4, including：First by polyether-polyamide block copolymer
It is dissolved in ethanol-water mixed solvent, adds nano silver slice, after mixing, is cast, is dried to obtain the mixed substrate membrane containing nano-grade molecular sieve.
6. preparation method according to claim 5, it is characterised in that：The nano silver slice passes through the side that comprises the following steps
Method is made：First silver nitrate and polyvinylpyrrolidone are added to the water, after dissolving, sequentially add sodium citrate, sodium borohydride,
Hydrogen peroxide and hydrazine hydrate, after the completion of reaction, isolated nano silver slice.
7. preparation method according to claim 6, it is characterised in that：The silver nitrate, polyvinylpyrrolidone and lemon
The mass ratio of sour sodium is 1:0.5:(0.1~0.09), the silver nitrate, sodium borohydride, the mol ratio of hydrogen peroxide and hydrazine hydrate are
1:0.001:(4.5~5):(4~4.5).
8. the application of mixed substrate membrane containing nano-grade molecular sieve described in claim 1, it is characterised in that：The mixed substrate membrane containing nano-grade molecular sieve is used for Selective Separation CO2
Gas.
9. application according to claim 8, it is characterised in that：The mixed substrate membrane containing nano-grade molecular sieve be used for UF membrane remove natural gas or
CO in biogas2Gas.
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| CN109865439A (en) * | 2019-01-22 | 2019-06-11 | 石河子大学 | A kind of mixed substrate membrane containing nano-grade molecular sieve and preparation method and application of the filling of ZIF-8/ graphite phase carbon nitride |
| CN110227361A (en) * | 2019-05-31 | 2019-09-13 | 太原理工大学 | A kind of preparation method and application of the mixed substrate membrane containing nano-grade molecular sieve of metakaolin and carbon nanotube modified synergic |
| CN111013409A (en) * | 2019-12-27 | 2020-04-17 | 天津工业大学 | Mixed matrix membrane filled with lanthanide fluoride porous nanosheets and preparation method and application thereof |
| CN112675720A (en) * | 2020-12-10 | 2021-04-20 | 石河子大学 | Preparation method and application of mixed matrix membrane filled with bimetallic strip material |
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