CN103933869A - Preparing method of ordered mesoporous carbon-stainless steel wire mesh composite separating membrane - Google Patents
Preparing method of ordered mesoporous carbon-stainless steel wire mesh composite separating membrane Download PDFInfo
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- CN103933869A CN103933869A CN201310023943.1A CN201310023943A CN103933869A CN 103933869 A CN103933869 A CN 103933869A CN 201310023943 A CN201310023943 A CN 201310023943A CN 103933869 A CN103933869 A CN 103933869A
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Abstract
The invention belongs to the fields of preparation of ordered mesoporous carbon materials and applications of the materials, and relates to a preparing method of an ordered mesoporous carbon-stainless steel wire mesh composite separating membrane. The preparing method includes: a step of cleaning and degreasing the surfaces of a carrier material; a step of dipping the carrier material into nitric acid to perform oxidation, and washing with distilled water until neutral; a step of adding a carbon source and a structure-directing agent into absolute ethanol and mixing, and stirring at room temperature uniformly to obtain a transparent solution; a step of putting the stainless steel wire mesh carrier material into the transparent solution to cover the carrier material with the solution so that a film-covered carrier material is obtained after volatilization at room temperature; and a step of ageing and calcinating. The composite separating membrane overcomes difficulties, namely difficult recovery and easy loss of traditional powder adsorbents and poor heat resistance of carrier materials. The composite separating membrane is simple in preparation process and has a wide prospect in the application field of pollutant separation.
Description
Technical field
The invention belongs to preparation and the application thereof of ordered mesoporous carbon material, relate to a kind of preparation method of ordered mesopore carbon-stainless steel cloth composite separating film.
Background technology
Mesoporous carbon is the novel non-silicon-based mesoporous material of a class, and having huge specific area (can be up to 2500m
2/ g) and pore volume (can be up to 2.25cm
3/ g), porosity is high, pore-size distribution is narrow, aperture is easy to regulate, surface, duct is easy to the features such as modification, therefore it demonstrates wide application prospect in fields such as catalysis, separation, medicine, environment, functional composite materials, becomes one of research frontier of multidisciplinary intersection.Meso-porous carbon material itself is powder, conventionally adopts suspension system in application process, and type of service is that meso-porous carbon material is sneaked in solution.Suspension system has with separated material and contacts the advantages such as abundant, but shortcoming is also apparent, because mesoporous carbon particle is very little, in use has easily cohesion, difficultly reclaims, loses the deficiencies such as large.For make mesoporous carbon convenient be applied to reality, research emphasis is focused on the immobilization research to mesoporous carbon by people.The Chinese patent application " a kind of method for making of ordered mesopore carbon-activated carbon fiber felt composite material and application " that is 201210236474.7 as application number proposes to use carbon fiber felt as matrix material, prepares in the above mesoporous carbon.But removing when template carbon fiber felt in high-temperature roasting can carbonization and frangible.Stainless steel cloth is conventionally selected as and separates prop carrier owing to having the large good characteristic such as large with intensity of loose structure, specific area, through the pretreated stainless steel cloth of surface oxidation, be easy to be combined with mesoporous carbon, thereby can be at the mesoporous carbon film of surface coverage one deck of stainless steel cloth, thereby reach the object of efficient separating contaminants.The work of preparing mesoporous carbon film at stainless steel wire net surface is a brand-new trial, at present, does not also have the research of this respect have not been reported.
Summary of the invention
Object of the present invention with a kind of method that ordered mesopore carbon-stainless steel cloth composite separating film is provided for the defect that overcomes prior art.
There is very big difference at the aspect such as physics, character in mesoporous carbon and stainless steel cloth, therefore the technical problem to be solved in the present invention is, overcomes deficiency of the prior art, taking stainless steel cloth as matrix material, with HNO
3solution carries out pretreatment to stainless steel surfaces, then utilize the method for evaporation induction self assembly (EISA) to prepare ordered mesopore carbon-stainless steel cloth composite separating film, and utilize the diffusion barrier preparing to carry out the separation application of multiple polluted-water, obtain desirable separating effect.
For achieving the above object, the present invention is by the following technical solutions:
A preparation method for ordered mesopore carbon-stainless steel cloth composite separating film, taking stainless steel cloth after pretreatment as matrix material, taking commercialization phenolic resins as carbon source, triblock copolymer (EO
106-PO
70-EO
106, F127) and be structure directing agent, utilize volatilization-induction self-assembling method to prepare ordered mesopore carbon-stainless steel cloth composite separating film.
A preparation method for ordered mesopore carbon-stainless steel cloth composite separating film, comprises the steps:
(1) carrier material is carried out to surface cleaning, oil removing;
(2) carrier material of surface clean step (1) being obtained is immersed in nitric acid and carries out oxidation processes, then uses distilled water to clean to neutral;
(3) by carbon source, structure directing agent, join in absolute ethyl alcohol (EtOH) and mix, under room temperature, stir and obtain clear solution, then the stainless steel cloth carrier material of the pretreated different meshes of step (2) is placed in to this clear solution and hangs and takes mixed solution, under room temperature, after volatilization, obtain biofilm carrier material;
(4) the biofilm carrier material after volatilization in step (3) is put into drying box aging;
(5) finally the biofilm carrier material after aging is placed in to roasting under nitrogen atmosphere, can obtains mesoporous carbon composite carrier high-efficient diffusion barrier.
Described carrier material is selected from the stainless steel cloth of different meshes.
Surface cleaning in described step (1) is by washed with de-ionized water, and oil removing adopts liquid detergent.
In described step (2), nitric acid is fuming nitric aicd, and oxidation treatment time is 24h.
In described step (3), carbon source is phenolic resins, and structure directing agent is F127, wherein carbon source: structure directing agent: the mass ratio of ethanol is=1:(1 ~ 1.5): (2 ~ 20).
The thickness that hangs and takes mixed solution in described step (3) is 10 μ m-200 μ m.
In described step (4), aging temperature is 100 ~ 150 DEG C, and ageing time is 12 ~ 24h.
In described step (5), nitrogen flow rate is 100ml/min, and sintering temperature is 350 ~ 900 DEG C, and the time is 6h.
The present invention has following beneficial effect:
The good characteristics such as the selected stainless steel cloth matrix material of the present invention is ductile, acid-alkali-corrosive-resisting, easy machine-shaping.Make stainless steel cloth surface nature that change occur by oxidation processes, be conducive to mesoporous carbon self assembly film forming in its surface.Ordered mesopore carbon-stainless steel cloth composite separating film prepared by the present invention has not only solved that conventional powder state adsorbent is difficult to reclaim, an easy difficult problem for loss and carrier material poor heat resistance, and preparation technology is simple, have broad prospects in the application aspect of separating contaminants.
Brief description of the drawings
Fig. 1 is the SEM photo of the stainless steel cloth base material that uses in the embodiment of the present invention.
Fig. 2 is the SEM photo of the ordered mesopore carbon-stainless steel cloth composite separating film in embodiment in the present invention
Fig. 3 is the TEM photo of the ordered mesopore carbon that scrapes on the stainless steel cloth base material in embodiment in the present invention
Detailed description of the invention
Below in conjunction with embodiment, technical scheme of the present invention is described further:
Stainless steel cloth matrix material is carried out to surface cleaning, oil removing work;
The stainless steel cloth of surface clean is immersed in to HNO
3in solution, carry out oxidation processes, then clean to neutral;
Taking commercialization phenolic resins (FR) as carbon source, F127 is structure directing agent, add absolute ethyl alcohol (EtOH) simultaneously, according to FR:F127:EtOH=1:(1 ~ 1.5): the mass ratio of (2 ~ 20) mixes, under room temperature, stir certain hour, pretreated stainless steel cloth is placed in to gained clear solution and hangs and takes certain thickness mixed liquor, under room temperature, volatilize;
Stainless steel cloth biofilm material after volatilization is put into the aging certain hour of drying box;
Finally the stainless steel cloth biofilm material after aging is placed in to roasting certain hour under nitrogen atmosphere, can obtains product.
Embodiment 1
(1) stainless steel cloth matrix material is carried out to surface cleaning, oil removing work;
(2) stainless steel cloth of surface clean step (1) being obtained is immersed in the HNO of being fuming
3in solution, carry out oxidation processes 12h, then carry out ultrasonic cleaning to neutral by deionized water;
(3) taking 2g F127 is structure directing agent, join 4g absolute ethyl alcohol (EtOH), under room temperature, be stirred to completely and dissolve, in ethanolic solution after dissolving, add 2g commercialization phenolic resins (FR) for carbon source (wherein, the mass ratio of FR:F127:EtOH is 1:1:2), then stir 1h and obtain clear solution, pretreated stainless steel cloth (100 order) is placed in to gained clear solution and hangs and takes secondary, under room temperature, after volatilization, obtain biofilm carrier material, mixed liquor thickness approximately 200 μ m;
(4) the stainless steel cloth biofilm material after volatilization is put into 100 DEG C of aging 12h of drying box;
(5) finally the stainless steel cloth biofilm material after aging is placed in to the lower 350 DEG C of roasting 6h of nitrogen atmosphere, wherein nitrogen flow rate is 100ml/min, can obtain product.
Wherein, Fig. 1 is the SEM photo of stainless steel cloth, and multiplication factor is 500 times, and each rhizoid Smooth is smooth.
Fig. 2 is the SEM photo of the ordered mesopore carbon-stainless steel cloth composite separating film in embodiment in the present invention.After the certain thickness mesoporous carbon of the online load of stainless steel wire, one deck carbon of can having seen Steel Wire Surface load.
Fig. 3 is the TEM photo of the mesoporous carbon that scrapes on the stainless steel cloth base material in embodiment in the present invention, in conjunction with obtaining mesoporous aperture in 2.5nm left and right after N2 absorption test, is the little and regular mesoporous carbon in a kind of aperture, efficiently separating contaminants.
Embodiment 2
(1) stainless steel cloth matrix material is carried out to surface cleaning, oil removing work;
(2) stainless steel cloth of surface clean step (1) being obtained is immersed in the HNO of being fuming
3in solution, carry out oxidation processes 12h, then carry out ultrasonic cleaning to neutral by deionized water;
(3) taking 2.4g F127 is structure directing agent, join 8g absolute ethyl alcohol (EtOH), under room temperature, be stirred to completely and dissolve, in ethanolic solution after dissolving, add 2g commercialization phenolic resins (FR) for carbon source (wherein, the mass ratio of FR:F127:EtOH is 1:1.2:8), stir again 1h and obtain clear solution, pretreated stainless steel cloth (800 order) is placed in to gained clear solution to be hung and taken twice, after volatilizing under room temperature, obtain biofilm carrier material, mixed liquor thickness is greatly about 50 μ m left and right;
(4) the stainless steel cloth biofilm material after volatilization is put into 110 DEG C of aging 12h of drying box;
(5) finally the stainless steel cloth biofilm material after aging is placed in to the lower 600 DEG C of roasting 6h of nitrogen atmosphere, wherein nitrogen flow rate is 100ml/min, can obtain product.
Embodiment 3
(1) stainless steel cloth matrix material is carried out to surface cleaning, oil removing work;
(2) stainless steel cloth of surface clean step (1) being obtained is immersed in the HNO of being fuming
3in solution, carry out oxidation processes 24h, then carry out ultrasonic cleaning to neutral by deionized water;
(3) taking 2.8g F127 is structure directing agent, join 12g absolute ethyl alcohol (EtOH), under room temperature, be stirred to completely and dissolve, in ethanolic solution after dissolving, add 2g commercialization phenolic resins (FR) for carbon source (wherein, the mass ratio of FR:F127:EtOH is 1:1.4:14), stir again 1h and obtain clear solution, pretreated stainless steel cloth (2000 order) is placed in to gained clear solution to be hung and taken three times, after volatilizing under room temperature, obtain biofilm carrier material, mixed liquor thickness approximately 80 μ m left and right;
(4) the stainless steel cloth biofilm material after volatilization is put into 130 DEG C of aging 24h of drying box;
(5) finally the stainless steel cloth biofilm material after aging is placed in to the lower 700 DEG C of roasting 6h of nitrogen atmosphere, wherein nitrogen flow rate is 100ml/min, can obtain product.
Embodiment 4
(1) stainless steel cloth matrix material is carried out to surface cleaning, oil removing work;
(2) stainless steel cloth of surface clean step (1) being obtained is immersed in the HNO of being fuming
3in solution, carry out oxidation processes 24h, then carry out ultrasonic cleaning to neutral by deionized water;
(3) taking 3g F127 is structure directing agent, join 16g absolute ethyl alcohol (EtOH), under room temperature, be stirred to completely and dissolve, in ethanolic solution after dissolving, add 2g commercialization phenolic resins (FR) for carbon source (wherein, the mass ratio of FR:F127:EtOH is 1:1.5:20), stir again 1h and obtain clear solution, pretreated stainless steel cloth (5000 order) is placed in to gained clear solution and hangs and takes mixed once liquid, after volatilizing under room temperature, obtain biofilm carrier material, mixed liquor thickness approximately 10 μ m left and right;
(4) the stainless steel cloth biofilm material after volatilization is put into 150 DEG C of aging 24h of drying box;
(5) finally the stainless steel cloth biofilm material after aging is placed in to the lower 900 DEG C of roasting 6h of nitrogen atmosphere, wherein nitrogen flow rate is 100ml/min, can obtain product.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.Person skilled in the art obviously can easily make various amendments to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not departing from improvement and the amendment that category of the present invention makes all should be within protection scope of the present invention.
Claims (8)
1. a preparation method for ordered mesopore carbon-stainless steel cloth composite separating film, is characterized in that: comprise the steps:
(1) carrier material is carried out to surface cleaning, oil removing;
(2) carrier material of surface clean step (1) being obtained is immersed in nitric acid and carries out oxidation processes, then uses distilled water to clean to neutral;
(3) by carbon source, structure directing agent, join in absolute ethyl alcohol and mix, under room temperature, stir and obtain clear solution, then the stainless steel cloth carrier material of the pretreated different meshes of step (2) is placed in to this clear solution and hangs and takes mixed solution, under room temperature, after volatilization, obtain biofilm carrier material;
(4) the biofilm carrier material after volatilization in step (3) is put into drying box aging;
(5) finally the biofilm carrier material after aging is placed in to roasting under nitrogen atmosphere, can obtains mesoporous carbon composite carrier high-efficient diffusion barrier.
2. preparation method according to claim 1, is characterized in that: described carrier material is selected from stainless steel cloth.
3. preparation method according to claim 1, is characterized in that: the surface cleaning in described step (1) is by washed with de-ionized water, and oil removing adopts liquid detergent.
4. preparation method according to claim 1, is characterized in that: in described step (2), nitric acid is fuming nitric aicd, and oxidation treatment time is 24h.
5. preparation method according to claim 1, it is characterized in that: in described step (3), carbon source is phenolic resins, structure directing agent is F127, wherein carbon source: structure directing agent: the mass ratio of ethanol is=1:(1 ~ 1.5): (2 ~ 20).
6. preparation method according to claim 1, is characterized in that: the thickness that hangs and takes mixed solution in described step (3) is 10 μ m-200 μ m.
7. preparation method according to claim 1, is characterized in that: in described step (4), aging temperature is 100 ~ 150 DEG C, and ageing time is 12 ~ 24h.
8. preparation method according to claim 1, is characterized in that: in described step (5), nitrogen flow rate is 100ml/min, and sintering temperature is 350 ~ 900 DEG C, and the time is 6h.
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| CN201310023943.1A CN103933869B (en) | 2013-01-23 | 2013-01-23 | A kind of preparation method of ordered mesopore carbon-stainless steel cloth composite separating film |
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|---|---|---|---|
| CN201310023943.1A CN103933869B (en) | 2013-01-23 | 2013-01-23 | A kind of preparation method of ordered mesopore carbon-stainless steel cloth composite separating film |
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| CN103933869A true CN103933869A (en) | 2014-07-23 |
| CN103933869B CN103933869B (en) | 2016-06-15 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104289114A (en) * | 2014-09-10 | 2015-01-21 | 同济大学 | Conductive filter membrane and application thereof |
| CN113067003A (en) * | 2019-12-14 | 2021-07-02 | 中国科学院大连化学物理研究所 | Fuel cell water guide plate and preparation method thereof |
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| CN1995458A (en) * | 2006-12-28 | 2007-07-11 | 赵蔚 | Method for promoting rustless steel surface hydrophilicity |
| CN102569842A (en) * | 2012-01-13 | 2012-07-11 | 南京航空航天大学 | Preparation method of hybrid ordered mesoporous carbon coat for protecting stainless steel bipolar plate of proton exchange membrane fuel cell |
| CN102580567A (en) * | 2011-12-31 | 2012-07-18 | 大连理工大学 | Composite carbon diaphragm with mesoporous and microporous gradient structure and preparation method for diaphragm |
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2013
- 2013-01-23 CN CN201310023943.1A patent/CN103933869B/en not_active Expired - Fee Related
Patent Citations (3)
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| CN1995458A (en) * | 2006-12-28 | 2007-07-11 | 赵蔚 | Method for promoting rustless steel surface hydrophilicity |
| CN102580567A (en) * | 2011-12-31 | 2012-07-18 | 大连理工大学 | Composite carbon diaphragm with mesoporous and microporous gradient structure and preparation method for diaphragm |
| CN102569842A (en) * | 2012-01-13 | 2012-07-11 | 南京航空航天大学 | Preparation method of hybrid ordered mesoporous carbon coat for protecting stainless steel bipolar plate of proton exchange membrane fuel cell |
Non-Patent Citations (2)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104289114A (en) * | 2014-09-10 | 2015-01-21 | 同济大学 | Conductive filter membrane and application thereof |
| CN104289114B (en) * | 2014-09-10 | 2016-10-19 | 同济大学 | A kind of conduction filter membrane and application thereof |
| CN113067003A (en) * | 2019-12-14 | 2021-07-02 | 中国科学院大连化学物理研究所 | Fuel cell water guide plate and preparation method thereof |
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| CN103933869B (en) | 2016-06-15 |
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