CN108479709A - A kind of preparation method of graphene Mayan indigo plant composite membrane - Google Patents
A kind of preparation method of graphene Mayan indigo plant composite membrane Download PDFInfo
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- CN108479709A CN108479709A CN201810526753.4A CN201810526753A CN108479709A CN 108479709 A CN108479709 A CN 108479709A CN 201810526753 A CN201810526753 A CN 201810526753A CN 108479709 A CN108479709 A CN 108479709A
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- indigo plant
- graphene oxide
- mayan indigo
- graphene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
- B01D53/02—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 adsorption, e.g. preparative gas chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
Abstract
The invention discloses a kind of preparation methods of graphene Mayan indigo plant composite membrane, graphene oxide, Mayan indigo plant nano particle are dispersed in water and organic solvent in the mixed solvent, prepare graphene oxide Mayan indigo plant dispersion liquid, by dispersion liquid concentration, freeze-drying, aeroge is prepared, aeroge is suppressed, film is prepared, film is heated and is restored, reduction film is prepared, then carbonized, activated, washed and obtain graphene Mayan indigo plant composite membrane.The blue compound film density in graphene Mayan that the present invention obtains is low, can the pernicious gases such as efficient absorption and decomposing formaldehyde, have application prospect in fields such as air purification, water process.
Description
Technical field
The invention belongs to grapheme material fields, are related to a kind of preparation method of graphene Mayan indigo plant composite membrane.
Background technology
The gases such as formaldehyde, sulfur dioxide, ammonia, nitric oxide are life and the polluted gas in industrial pollution.In particular, room
Interior formaldehyde in air has become the major pollutants for influencing human health, harm of the formaldehyde to human body in winter air
It is especially big, to the apparent stimulation of the generations such as eye, nose, larynx and skin.Absorption method is air as a kind of physico-chemical process
A kind of one of important method in purification has the advantages such as of low cost, removal efficiency is high, non-secondary pollution, easy regeneration.It is numerous
In sorbing material, carbon material is a kind of sorbing material being most widely used.
Activated carbon is the most commonly used methyl aldehyde adsorption material, since it is with abundant pore structure, high specific surface area and
Surface-active, can effective pernicious gases such as formaldehyde adsorption.But the time of equilibrium adsorption of activated carbon is short, and it is flat to reach absorption soon
Weighing apparatus, it is ineffective.In addition, under heating condition, formaldehyde can be released from activated carbon, therefore after activated carbon adsorption balance
It handles not in time, activated carbon possibly even becomes the source of release of formaldehyde.Many people are conceived to the modification to activated carbon in recent years, but
Also it only is confined to the property of itself, such as improves surface-active, increase porosity to improve adsorption rate.But how efficiently by first
Aldehyde decomposition is still a great problem.
Invention content
The purpose of the present invention is insufficient in view of the prior art, a kind of preparation side of graphene Mayan indigo plant composite membrane is provided
Method.
The purpose of the present invention is what is be achieved through the following technical solutions：
(1) graphene oxide, Mayan indigo plant nano particle are dispersed in water and organic solvent in the mixed solvent, prepare oxidation stone
Black alkene Mayan indigo plant dispersion liquid；
(2) by the concentration of graphene oxide Mayan indigo plant dispersion liquid, freeze-drying, graphene oxide Mayan indigo plant aeroge is prepared；
(3) graphene oxide Mayan indigo plant aeroge is suppressed, graphene oxide Mayan indigo plant film is prepared；
(4) graphene oxide Mayan indigo plant film is heated and is restored, reduced graphene Mayan indigo plant film is prepared；
(5) composite membrane that step (4) obtains carbonized, activated, washed and obtain graphene Mayan indigo plant composite membrane.
Further, in step (1), the mass ratio of graphene oxide and Mayan indigo plant nano particle is 10：1~20：1.
Further, in step (1), the organic solvent is one or more of mixed in methanol, ethyl alcohol, propyl alcohol or butanol
It closes.
Further, in step (1), the volume ratio of the water and organic solvent is 100：1~100：15.
Further, in step (2), the concentration is using the method for vacuum distillation, the quality after concentration dispersion liquid concentration
Score is 15wt%~25wt%.
Further, in step (2), the temperature of the freeze-drying is -30 DEG C~-60 DEG C, and the time of freeze-drying is
38h~76h.
Further, in step (3), the thickness of graphene oxide membrane is 100nm~200nm after compacting.
Further, in step (4), the heating temperature of the heating reduction of graphene oxide membrane is 210 DEG C~250 DEG C；Add
The thermal reduction time is 5min~30min.
Further, the carbonization temperature described in step (5) is 350~500 DEG C, and carbonization time is 2~7h, activation temperature
It it is 600~900 DEG C, soak time is 2~4h.
Gained graphene Mayan of the invention indigo plant composite membrane has high-specific surface area, high porosity and low-density, and stability is good,
It can effectively adsorb and the formaldehyde in air of degrading, can be used for the fields such as air purification, water process, catalytic carrier, electrochemical material.
Specific implementation mode
Further below by embodiment with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary concrete numerical value.
Embodiment 1：
(1) graphene oxide, Mayan indigo plant nano particle are dispersed in water and organic solvent in the mixed solvent, prepare oxidation stone
Black alkene Mayan indigo plant dispersion liquid；
(2) by the concentration of graphene oxide Mayan indigo plant dispersion liquid, freeze-drying, graphene oxide Mayan indigo plant aeroge is prepared；
(3) graphene oxide Mayan indigo plant aeroge is suppressed, graphene oxide Mayan indigo plant film is prepared；
(4) graphene oxide Mayan indigo plant film is heated and is restored, reduced graphene Mayan indigo plant film is prepared；
(5) composite membrane that step (4) obtains carbonized, activated, washed and obtain graphene Mayan indigo plant composite membrane.
Wherein, in step (1), the mass ratio of graphene oxide and Mayan indigo plant nano particle is 10：1, the organic solvent
Selected from methanol, the volume ratio of the water and organic solvent is 100：1；In step (2), the concentration is using the side being evaporated under reduced pressure
Method, the mass fraction after concentration dispersion liquid concentration are 15wt%, and the temperature of the freeze-drying is -30 DEG C, freeze-drying when
Between be 38h；In step (3), the thickness of graphene oxide membrane is 100nm after compacting；In step (4), graphene oxide membrane adds
The heating temperature of thermal reduction is 210 DEG C；The heating recovery time is 5min；Carbonization temperature described in step (5) is 350, charing
Time is 2h, and activation temperature is 600 DEG C, soak time 2h.
Through above step, obtained graphene Mayan indigo plant composite membrane is degraded under the formaldehyde atmosphere of 100ppm after illumination 8h
Rate is 72%.
Embodiment 2：
(1) graphene oxide, Mayan indigo plant nano particle are dispersed in water and organic solvent in the mixed solvent, prepare oxidation stone
Black alkene Mayan indigo plant dispersion liquid；
(2) by the concentration of graphene oxide Mayan indigo plant dispersion liquid, freeze-drying, graphene oxide Mayan indigo plant aeroge is prepared；
(3) graphene oxide Mayan indigo plant aeroge is suppressed, graphene oxide Mayan indigo plant film is prepared；
(4) graphene oxide Mayan indigo plant film is heated and is restored, reduced graphene Mayan indigo plant film is prepared；
(5) composite membrane that step (4) obtains carbonized, activated, washed and obtain graphene Mayan indigo plant composite membrane.
Wherein, in step (1), the mass ratio of graphene oxide and Mayan indigo plant nano particle is 20：1, the organic solvent
Selected from ethyl alcohol, the volume ratio of the water and organic solvent is 100：15；In step (2), the concentration is using the side being evaporated under reduced pressure
Method, the mass fraction after concentration dispersion liquid concentration are 25wt%, and the temperature of the freeze-drying is -60 DEG C, freeze-drying when
Between be 76h；In step (3), the thickness of graphene oxide membrane is 200nm after compacting；In step (4), graphene oxide membrane adds
The heating temperature of thermal reduction is 250 DEG C；The heating recovery time is 30min；Carbonization temperature described in step (5) is 500 DEG C, charcoal
The change time is 7h, and activation temperature is 900 DEG C, soak time 4h.
Through above step, obtained graphene Mayan indigo plant composite membrane is degraded under the formaldehyde atmosphere of 100ppm after illumination 8h
Rate is 75%.
Embodiment 3：
(1) graphene oxide, Mayan indigo plant nano particle are dispersed in water and organic solvent in the mixed solvent, prepare oxidation stone
Black alkene Mayan indigo plant dispersion liquid；
(2) by the concentration of graphene oxide Mayan indigo plant dispersion liquid, freeze-drying, graphene oxide Mayan indigo plant aeroge is prepared；
(3) graphene oxide Mayan indigo plant aeroge is suppressed, graphene oxide Mayan indigo plant film is prepared；
(4) graphene oxide Mayan indigo plant film is heated and is restored, reduced graphene Mayan indigo plant film is prepared；
(5) composite membrane that step (4) obtains carbonized, activated, washed and obtain graphene Mayan indigo plant composite membrane.
Wherein, in step (1), the mass ratio of graphene oxide and Mayan indigo plant nano particle is 15：1, the organic solvent
Selected from propyl alcohol, the volume ratio of the water and organic solvent is 100：10；In step (2), the concentration is using the side being evaporated under reduced pressure
Method, the mass fraction after concentration dispersion liquid concentration are 20wt%, and the temperature of the freeze-drying is -50 DEG C, freeze-drying when
Between be 58h；In step (3), the thickness of graphene oxide membrane is 150nm after compacting；In step (4), graphene oxide membrane adds
The heating temperature of thermal reduction is 230 DEG C；The heating recovery time is 20min；Carbonization temperature described in step (5) is 400 DEG C, charcoal
The change time is 5h, and activation temperature is 800 DEG C, soak time 3h.
Through above step, obtained graphene Mayan indigo plant composite membrane is degraded under the formaldehyde atmosphere of 100ppm after illumination 8h
Rate is 78%.
Comparative example 1：
(1) graphene oxide, activated carbon nano particle are dispersed in water and organic solvent in the mixed solvent, prepare oxidation stone
Black alkene activated carbon dispersion liquid；
(2) by the concentration of graphene oxide activated carbon dispersion liquid, freeze-drying, graphene oxide activity charcoal-aero gel is prepared；
(3) graphene oxide activity charcoal-aero gel is suppressed, graphene oxide activated charcoal membrane is prepared；
(4) magnesium oxide/absorbent charcoal graphene film is heated and is restored, reduced graphene active carbon composite membrane is prepared；
(5) composite membrane that step (4) obtains carbonized, activated, washed and obtain graphene active carbon composite membrane.
Wherein, in step (1), the mass ratio of graphene oxide and activated carbon nano particle is 15：1, the organic solvent
Selected from propyl alcohol, the volume ratio of the water and organic solvent is 100：10；In step (2), the concentration is using the side being evaporated under reduced pressure
Method, the mass fraction after concentration dispersion liquid concentration are 20wt%, and the temperature of the freeze-drying is -50 DEG C, freeze-drying when
Between be 58h；In step (3), the thickness of graphene oxide membrane is 150nm after compacting；In step (4), graphene oxide membrane adds
The heating temperature of thermal reduction is 230 DEG C；The heating recovery time is 20min；Carbonization temperature described in step (5) is 400 DEG C, charcoal
The change time is 5h, and activation temperature is 800 DEG C, soak time 3h.
Through above step, obtained graphene active carbon composite membrane is degraded under the formaldehyde atmosphere of 100ppm after illumination 8h
Rate is 58%.
Comparative example 2
(1) graphene oxide, activated carbon nano particle are dispersed in water and organic solvent in the mixed solvent, prepare oxidation stone
Black alkene activated carbon dispersion liquid；
(2) by the concentration of graphene oxide activated carbon dispersion liquid, freeze-drying, graphene oxide activity charcoal-aero gel is prepared；
(3) graphene oxide activity charcoal-aero gel is suppressed, graphene oxide activated charcoal membrane is prepared；
(4) magnesium oxide/absorbent charcoal graphene film is heated and is restored, reduced graphene active carbon composite membrane is prepared；
(5) composite membrane that step (4) obtains carbonized, activated, washed and obtain graphene active carbon composite membrane.
Wherein, in step (1), the mass ratio of graphene oxide and activated carbon nano particle is 10：1, the organic solvent
Selected from methanol, the volume ratio of the water and organic solvent is 100：1；In step (2), the concentration is using the side being evaporated under reduced pressure
Method, the mass fraction after concentration dispersion liquid concentration are 15wt%, and the temperature of the freeze-drying is -30 DEG C, freeze-drying when
Between be 38h；In step (3), the thickness of graphene oxide membrane is 100nm after compacting；In step (4), graphene oxide membrane adds
The heating temperature of thermal reduction is 210 DEG C；The heating recovery time is 5min；Carbonization temperature described in step (5) is 350, charing
Time is 2h, and activation temperature is 600 DEG C, soak time 2h.
Through above step, obtained graphene active carbon composite membrane is degraded under the formaldehyde atmosphere of 100ppm after illumination 8h
Rate is 62%.
Graphene Mayan indigo plant composite membrane made of the present invention achieves aobvious relative to existing graphene active carbon composite membrane
The effect of work.
Although the above-mentioned specific implementation mode to the present invention is described, not to the limit of the scope of the present invention
System, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art need not pay
It is still within the scope of the present invention to go out the various modifications or changes that creative work can be made.
Claims (9)
1. a kind of preparation method of graphene Mayan indigo plant composite membrane, includes the following steps：
(1) graphene oxide, Mayan indigo plant nano particle are dispersed in water and organic solvent in the mixed solvent, prepare graphene oxide
Mayan indigo plant dispersion liquid；
(2) by the concentration of graphene oxide Mayan indigo plant dispersion liquid, freeze-drying, graphene oxide Mayan indigo plant aeroge is prepared；
(3) graphene oxide Mayan indigo plant aeroge is suppressed, graphene oxide Mayan indigo plant film is prepared；
(4) graphene oxide Mayan indigo plant film is heated and is restored, reduced graphene Mayan indigo plant film is prepared；
(5) composite membrane that step (4) obtains carbonized, activated, washed and obtain graphene Mayan indigo plant composite membrane.
2. preparation method according to claim 1, which is characterized in that in step (1), graphene oxide and Mayan indigo plant nanometer
The mass ratio of particle is 10：1~20：1.
3. preparation method according to claim 1, which is characterized in that in step (1), the organic solvent be selected from methanol,
One or more of mixing in ethyl alcohol, propyl alcohol or butanol.
4. preparation method according to claim 1, which is characterized in that in step (1), the volume of the water and organic solvent
Than being 100：1~100：15.
5. preparation method according to claim 1, which is characterized in that in step (2), the concentration is using vacuum distillation
Method, the mass fraction after concentration dispersion liquid concentration is 15wt%~25wt%.
6. preparation method according to claim 1, which is characterized in that in step (2), the temperature of the freeze-drying is-
30 DEG C~-60 DEG C, the time of freeze-drying is 38h~76h.
7. according to claim 1-6 any one of them preparation methods, which is characterized in that in step (3), graphite oxide after compacting
The thickness of alkene film is 100nm~200nm.
8. preparation method according to claim 7, which is characterized in that in step (4), the heating of graphene oxide membrane restores
Heating temperature be 210 DEG C~250 DEG C；The heating recovery time is 5min~30min.
9. according to the method described in claim 8, it is characterized in that, carbonization temperature described in step (5) is 350~500 DEG C,
Carbonization time is 2~7h, and activation temperature is 600~900 DEG C, and soak time is 2~4h.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102367570A (en) * | 2011-11-01 | 2012-03-07 | 南昌航空大学 | Method for preparing diamond-graphene composite film |
| CN106986408A (en) * | 2017-05-03 | 2017-07-28 | 西安航空学院 | A kind of high efficiency sewage treating agent and preparation method thereof |
| CN107091499A (en) * | 2017-05-12 | 2017-08-25 | 程艳青 | A kind of multi-staged air cleaning system |
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| CN107381544A (en) * | 2017-06-16 | 2017-11-24 | 中国科学院福建物质结构研究所 | A kind of graphene film and its preparation method and application |
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2018
- 2018-05-29 CN CN201810526753.4A patent/CN108479709A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102367570A (en) * | 2011-11-01 | 2012-03-07 | 南昌航空大学 | Method for preparing diamond-graphene composite film |
| CN106986408A (en) * | 2017-05-03 | 2017-07-28 | 西安航空学院 | A kind of high efficiency sewage treating agent and preparation method thereof |
| CN107091499A (en) * | 2017-05-12 | 2017-08-25 | 程艳青 | A kind of multi-staged air cleaning system |
| CN107381544A (en) * | 2017-06-16 | 2017-11-24 | 中国科学院福建物质结构研究所 | A kind of graphene film and its preparation method and application |
| CN107243255A (en) * | 2017-06-20 | 2017-10-13 | 杭州牛墨科技有限公司 | A kind of finishing pollution sweep-out method |
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