CN108295671A - A kind of application of two dimension MXene films in water and isopropanol separation - Google Patents
A kind of application of two dimension MXene films in water and isopropanol separation Download PDFInfo
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- CN108295671A CN108295671A CN201810099040.4A CN201810099040A CN108295671A CN 108295671 A CN108295671 A CN 108295671A CN 201810099040 A CN201810099040 A CN 201810099040A CN 108295671 A CN108295671 A CN 108295671A
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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
- B01D71/024—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/08—Thickening liquid suspensions by filtration
- B01D17/085—Thickening liquid suspensions by filtration with membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/36—Pervaporation; Membrane distillation; Liquid permeation
- B01D61/362—Pervaporation
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Abstract
The invention discloses a kind of application of two dimension MXene films in water and isopropanol separation, belong to two-dimensional nano membrane preparation technology and liquid separation technology field.The application includes the following steps：（1）Two-dimentional MXene films are put into infiltration evaporation device, isopropanol water solution is added in feed side；（2）Per-meate side is vacuumized using vacuum pump, and the steam of infiltration is passed through in cold-trap and is condensed；（3）The penetrating fluid in cold-trap is collected, the concentration of gas chromatographic detection penetrating fluid is used in combination.Two-dimentional MXene films with good mechanical performance and excellent separating property are put into infiltration evaporation device by the present invention, separation for water and isopropanol, with very high selectivity and good chemical stability, there is commercial application potentiality in liquid separation field.
Description
Technical field
The invention belongs to nanometer films and liquid separation technology field, and in particular to a kind of two dimension MXene films are in water and isopropyl
Application in alcohol separation.
Background technology
As global resources are in short supply, environmental pollution form getting worse, people constantly pursue energy-efficient chemical industry life
Production mode.Separation is a highly important link in chemical process.In liquid separation field, traditional point such as rectifying
Complicated for operation from method, energy consumption is huge.And the membrane separating method advantage that last decade is risen is notable, can substantially reduce energy consumption, improves
Separative efficiency becomes the new direction of future development.
Isopropanol is a kind of important industrial chemicals, is used primarily in the fields such as medicine, cosmetics, plastics, fragrance, coating.
Isopropanol seemingly, can be dissolved in water, and form azeotropic mixture with water when mass concentration is 87.9%, this makes due to polarity and water phase
We are difficult that anhydrous isopropyl alcohol is prepared by general rectification method.Traditional solution is using azeotropic distillation, absorption
Rectifying or extracting rectifying, these methods need to additionally incorporate azeotropic mixture, adsorbent or extractant so that process is complicated, energy consumption
It is huge.Water and isopropanol are detached according to membrane separating method, separative efficiency can be greatly promoted, reduces energy consumption.Achievable quotient at present
The traditional liquid seperation film of industry has polymer film and molecular screen membrane, and that there are stability is bad for they, and selectivity and penetration are difficult to
The defects of taking into account.Therefore, developing the liquid separating film of novel high quality becomes a big research hotspot in UF membrane field.
In recent years, graphene oxide membrane achieves many progress, similar two-dimensional nano in the application of liquid separation field
Membrane material because its satisfactory mechanical property, chemical stability is high, it is simple to prepare, have excellent performance the features such as cause the extensive pass of scientific research circle
Note.A kind of nearest neoteric two dimension MXene films prepare simpler, electric conductivity higher compared with graphene oxide membrane, hydrophilic
Property is more preferable, and commercial application potentiality has been shown in separation field.
Invention content
The shortcomings that in order to improve the prior art, realizes that breakthrough of the MXene films in liquid separation field, the purpose of the present invention exist
In a kind of application of the two dimension MXene films of offer in water and isopropanol separation.
The purpose of the present invention is achieved through the following technical solutions.
A kind of application of two dimension MXene films in water and isopropanol separation, includes the following steps：
（1）Two-dimentional MXene films are put into commercial infiltration evaporation device, the isopropanol that various concentration is added in feed side is water-soluble
Liquid；
（2）Per-meate side is vacuumized using vacuum pump, and the steam of infiltration is passed through in cold-trap and is condensed；
（3）The quality for weighing the penetrating fluid in cold-trap, is used in combination its concentration of gas chromatographic detection, you can obtain various concentration isopropanol
The penetration and selectivity of aqueous solution.
Preferably, step（1）The thickness of the two dimension MXene films is 10nm ~ 10mm.
Preferably, step（1）The mass concentration of the isopropanol water solution is 5% ~ 96%.
Preferably, step（2）The vacuum degree of the per-meate side is -0.94 ~ -0.1MPa, further preferably -0.1MPa.
Preferably, step（2）The cold-trap reduces temperature using liquid nitrogen.
Preferably, step（2）The temperature of the cold-trap is -196 DEG C.
Preferably, step（3）The gas-chromatography is Agilent 7890A gas-chromatographies.
Preferably, step（1）The preparation method of the two dimension MXene films, includes the following steps：
（1）Villiaumite is added in hydrochloric acid solution, is stirred evenly, MAX powder is added, is stirred to react, is centrifuged, is washed, it is dry, it obtains
MXene powder；
（2）MXene powder after etching is scattered in solvent, is centrifuged after supersound process, takes its supernatant, you can obtain
MXene two-dimensional nano piece solution；
（3）By step（2）The solution of the MXene nanometer sheets of gained is dried to obtain using on vacuum filtration to nylon66 fiber substrate
MXene films.
It is further preferred that step（1）Described in MAX powder be Ti2AlC、V2AlC、Ti3SiC2、Ti3AlC2、
Ti4AlN3And Nb4AlC3In one kind.
It is further preferred that step（3）Described in contain two dimension MXene nanometer sheet solution a concentration of 0.1 ~ 10 mg/
ml。
It is further preferred that step（3）Described in nylon66 fiber substrate aperture be 0.2 μm, a diameter of 50mm.By above
A kind of two dimension MXene films, surface made from the method do not have crack, have good flexibility and mechanical performance.
A kind of two dimension MXene films of the present invention are detached for water and isopropanol, have higher penetration and selectivity,
Industrially there is prodigious application value.
Compared with prior art, the invention has the advantages that and advantageous effect：
（1）Two-dimentional MXene films are used for water and when efficiently separating of isopropanol by the present invention, have very high penetration and selectivity,
With commercial application potentiality.
（2）Two-dimentional MXene film preparations used in the present invention are simple, at low cost, are suitble to industrialization large-scale production.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Embodiment 1
A kind of preparation method of two dimension MXene films, includes the following steps：
（1）200mL 6molL are added in 8g lithium fluoride-1Hydrochloric acid solution in, stir evenly, add 5gTi3AlC2Powder,
It is stirred to react 48h, centrifuge washing under the conditions of 2500rpm, until upper layer solution PH is in neutrality, then drying 48 is small at 50 DEG C
When, obtain Ti3C2Powder；
（2）By 0.1g Ti3C2Powder is added in 500mL deionized waters, and ultrasound 1 hour centrifuges 1 hour at 2500rpm, inhales
Supernatant liquid is taken to obtain the solution of two-dimentional MXene nanometer sheets, a concentration of 0.1mg/mL；
（3）Take 10mL steps（2）MXene nanometer sheets are stacked by gained MXene nanometer sheet solution using Vacuum filtration device
Aperture is 200nm, then 10 hours dry in 100 DEG C of air dry ovens in the nylon66 fiber substrate of a diameter of 50mm, obtains thickness
Degree is the two-dimentional MXene films of 10nm.
Application of the two-dimentional MXene films of the present embodiment in water and isopropanol separation：
By thickness be 10nm two-dimentional MXene films be put into infiltration evaporation device, feed side be added mass concentration be 5% it is different
Aqueous propanol solution；Per-meate side is evacuated to by -0.094MPa using vacuum pump, and it is -196 DEG C that the steam of infiltration, which is passed through temperature,
Cold-trap in condense；The penetrating fluid in cold-trap is collected, its quality is weighed, Agilent 7890A gas chromatographic detection penetrating fluids is used in combination
Concentration.
Total penetration that experiment measures 5% isopropanol water solution is 1825 gm2·h-1, selectivity is 72.Illustrating will be two-dimentional
MXene films are in water and isopropanol separation, having very high penetration and selectivity, industrially there is prodigious application value.
Embodiment 2
A kind of preparation method of two dimension MXene films, includes the following steps：
（1）200mL 6molL are added in 8g lithium fluoride-1Hydrochloric acid solution in, stir evenly, add 5gTi3AlC2Powder,
It is stirred to react 48h, centrifuge washing under the conditions of 2500rpm, until upper layer solution PH is in neutrality, then drying 48 is small at 50 DEG C
When, obtain Ti3C2Powder；
（2）By 3g Ti3C2Ultrasound 1 hour in 500mL deionized waters is added in powder, is centrifuged 1 hour at 2500rpm, in absorption
Layer liquid obtains the solution of two-dimentional MXene nanometer sheets, a concentration of 5mg/mL；
（3）Take 50mL steps（2）MXene nanometer sheets are stacked by gained MXene nanometer sheet solution using Vacuum filtration device
Aperture is 200nm, then 10 hours dry in 100 DEG C of air dry ovens in the nylon66 fiber substrate of a diameter of 50mm, obtains thickness
Degree is 5mm two dimension MXene films.
Application of the two-dimentional MXene films of the present embodiment in water and isopropanol separation：
By thickness be 5mm two-dimentional MXene films be put into infiltration evaporation device, feed side be added mass concentration be 50% it is different
Aqueous propanol solution；Per-meate side is evacuated to by -0.96MPa using vacuum pump, and it is -196 DEG C that the steam of infiltration, which is passed through temperature,
Cold-trap in condense；The penetrating fluid in cold-trap is collected, its quality is weighed, Agilent 7890A gas chromatographic detection penetrating fluids is used in combination
Concentration.
Total penetration that experiment measures 50% isopropanol water solution is 964 gm2·h-1, selectivity is 90.Illustrating will be two-dimentional
MXene films are in water and isopropanol separation, having very high penetration and selectivity.Industrially there is prodigious application value.
Embodiment 3
A kind of preparation method of two dimension MXene films, includes the following steps：
（1）200mL 6molL are added in 8g lithium fluoride-1Hydrochloric acid solution in, stir evenly, add 5gTi3AlC2Powder,
It is stirred to react 48h, centrifuge washing under the conditions of 2500rpm, until upper layer solution PH is in neutrality, then drying 48 is small at 50 DEG C
When, obtain Ti3C2Powder；
（2）By 10g Ti3C2Powder is added in 500mL deionized waters, and ultrasound 1 hour centrifuges 1 hour at 2500rpm, draws
Supernatant liquid obtains the solution of two-dimentional MXene nanometer sheets, a concentration of 15mg/mL；
（3）Take 50mL steps（2）MXene nanometer sheets are stacked by gained MXene nanometer sheet solution using Vacuum filtration device
Aperture is 200nm, then 10 hours dry in 150 DEG C of air dry ovens in the nylon66 fiber substrate of a diameter of 50mm, obtains thickness
Degree is the two-dimentional MXene films of 10mm.
Application of the two-dimentional MXene films of the present embodiment in water and isopropanol separation：
By thickness be 10mm two-dimentional MXene films be put into infiltration evaporation device, feed side be added mass concentration be 96% it is different
Aqueous propanol solution；Per-meate side is evacuated to by -0.96MPa using vacuum pump, and it is -196 DEG C that the steam of infiltration, which is passed through temperature,
Cold-trap in condense；The penetrating fluid in cold-trap is collected, its quality is weighed, Agilent 7890A gas chromatographic detection penetrating fluids is used in combination
Concentration.
Total penetration that experiment measures 96% isopropanol water solution is divided into 532 gm2·h-1, selectivity is 178.Illustrate two
MXene films are tieed up in water and isopropanol separation, there is very high penetration and selectivity, industrially there is prodigious application value.
Claims (6)
1. a kind of application of two dimension MXene films in water and isopropanol separation, which is characterized in that include the following steps：
（1）Two-dimentional MXene films are put into infiltration evaporation device, isopropanol water solution is added in feed side；
（2）The per-meate side of infiltration evaporation device is vacuumized using vacuum pump, and the steam of infiltration is passed through in cold-trap and is condensed；
（3）The penetrating fluid in cold-trap is collected, the concentration of gas chromatographic detection penetrating fluid is used in combination.
2. application according to claim 1, which is characterized in that step（1）The thickness of the two dimension MXene films be 10nm ~
10mm。
3. application according to claim 1, which is characterized in that step（1）The mass concentration of the isopropanol water solution is
5%~96%。
4. application according to claim 1, which is characterized in that step（2）The vacuum degree of the per-meate side be -0.94 ~ -
0.1MPa。
5. application according to claim 1, which is characterized in that step（2）The cold-trap reduces temperature using liquid nitrogen.
6. application according to claim 1, which is characterized in that step（2）The temperature of the cold-trap is -196 DEG C.
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| CN201810099040.4A CN108295671A (en) | 2018-01-31 | 2018-01-31 | A kind of application of two dimension MXene films in water and isopropanol separation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109569319A (en) * | 2018-12-14 | 2019-04-05 | 华南理工大学 | A kind of application of the two dimension self-crosslinking MXene film in ion isolation |
| CN111017890A (en) * | 2019-12-30 | 2020-04-17 | 哈尔滨工业大学 | Method for rapidly preparing MXene film with high volume specific capacitance |
Citations (4)
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| JPS5884005A (en) * | 1981-11-13 | 1983-05-20 | Asahi Glass Co Ltd | Separating method for liquid mixture |
| CN106178979A (en) * | 2016-08-31 | 2016-12-07 | 华南理工大学 | High-performance two-dimensional stratiform Ti3c2mXene film and preparation method thereof and the application in water process |
| CN106457159A (en) * | 2014-05-08 | 2017-02-22 | 洛克希德马丁公司 | Stacked two-dimensional materials and methods for producing structures incorporating same |
| CN106477578A (en) * | 2015-08-27 | 2017-03-08 | 大连理工大学 | A kind of MXene two-dimensional material preparation method based on acid deep co-melting solvent |
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2018
- 2018-01-31 CN CN201810099040.4A patent/CN108295671A/en active Pending
Patent Citations (4)
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|---|---|---|---|---|
| JPS5884005A (en) * | 1981-11-13 | 1983-05-20 | Asahi Glass Co Ltd | Separating method for liquid mixture |
| CN106457159A (en) * | 2014-05-08 | 2017-02-22 | 洛克希德马丁公司 | Stacked two-dimensional materials and methods for producing structures incorporating same |
| CN106477578A (en) * | 2015-08-27 | 2017-03-08 | 大连理工大学 | A kind of MXene two-dimensional material preparation method based on acid deep co-melting solvent |
| CN106178979A (en) * | 2016-08-31 | 2016-12-07 | 华南理工大学 | High-performance two-dimensional stratiform Ti3c2mXene film and preparation method thereof and the application in water process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109569319A (en) * | 2018-12-14 | 2019-04-05 | 华南理工大学 | A kind of application of the two dimension self-crosslinking MXene film in ion isolation |
| CN109569319B (en) * | 2018-12-14 | 2021-12-21 | 华南理工大学 | Application of two-dimensional self-crosslinking MXene membrane in ion separation |
| CN111017890A (en) * | 2019-12-30 | 2020-04-17 | 哈尔滨工业大学 | Method for rapidly preparing MXene film with high volume specific capacitance |
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Application publication date: 20180720 |
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