CN110255523A - A kind of preparation method of carbon-based photothermal conversion film - Google Patents

A kind of preparation method of carbon-based photothermal conversion film Download PDF

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Publication number
CN110255523A
CN110255523A CN201810202023.9A CN201810202023A CN110255523A CN 110255523 A CN110255523 A CN 110255523A CN 201810202023 A CN201810202023 A CN 201810202023A CN 110255523 A CN110255523 A CN 110255523A
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China
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carbon
photothermal conversion
degrees celsius
conversion film
preparation
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CN201810202023.9A
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Chinese (zh)
Inventor
于一夫
陈亚西
张兵
黄义
史艳梅
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Tianjin University
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Tianjin University
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/05Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/14Treatment of water, waste water, or sewage by heating by distillation or evaporation using solar energy
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A20/00Water conservation; Efficient water supply; Efficient water use
    • Y02A20/20Controlling water pollution; Waste water treatment
    • Y02A20/208Off-grid powered water treatment
    • Y02A20/212Solar-powered wastewater sewage treatment, e.g. spray evaporation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The present invention discloses a kind of preparation method of carbon-based photothermal conversion film, and paper is carried out heating carbonization in inert protective atmosphere, to obtain carbon-based photothermal conversion film.Judge that by the whole components of carbonization rear film, paper is changed into obvious hydrophobicity by water imbibition after carbonization for carbon by EDS, and when as carbon-based photothermal conversion film, shows excellent performance.

Description

A kind of preparation method of carbon-based photothermal conversion film
Technical field
The present invention relates to optical-thermal conversion material technical fields, are about a kind of carbon-based water evaporation film more particularly Preparation method.
Background technique
In nature, water evaporation is the important component of earth water circulation.The radiation of the sun is that water is converted into water steaming Gas important impetus.Because water is converted into the process that vapor is a heat absorption, solar energy is exactly the heat source of water gas shift. In nature, solar irradiation is mapped to the surface in mountains and rivers lake, directly heats to water body, and the movement for accelerating hydrone increases The speed that hydrone is overflowed from liquid gas meter face, to form the process of photic water evaporation.This process finds and utilized by the mankind, Drinkable fresh water is obtained using solar distilling during human evolution to sustain life.With the quick hair of modern industry Exhibition, we are faced with increasingly severe water pollution problems.Seawater is handled using solar energy highly effective and industrial wastewater generates cleaning Water is a up-and-coming approach for solving the problems, such as shortage of water resources.However, naturally water evaporation is not able to satisfy specific ring The solar distilling in border obtains the demand of fresh water.Evaporation is the process occurred in liquid gas meter face in fact.The sun in nature Heating evaporation is carried out to water, is heated to the entirety of water, if it is possible to improve sunlight to liquid gas surface water layer in part Heating would be even more beneficial to quickening water and be converted into vapor.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of one-step method to be prepared, and cellulose is thin Film direct carbonization forms the carbon film material of integraty, constructs carbon-based photothermal conversion system, realizes optothermal material integration, a step The method that metaplasia produces carbon-based photothermal conversion system makes full use of existing paper to carry out deep processing and exploitation.
Technical purpose of the invention is achieved by following technical proposals:
The preparation facilities equipment of carbon-based photothermal conversion film, including inner and outer tubes, the table in inner tube outer surface and outer tube Support member is set between face, so that inner and outer tubes are coaxially disposed to form tube-in-tube structure, the outer surface of inner tube is arranged in paper handkerchief On, i.e., application of the above-mentioned preparation facilities equipment in the preparation of carbon-based photothermal conversion film.
Furtherly, both ends of the inner tube, paper handkerchief is arranged in outside the inner tube between two-end support parts for support member setting On surface.
Furtherly, support member is circumferentially uniformly distributed, and preferably 2-6.
Furtherly, support member is metallic support, and outer tube and inner tube select quartz ampoule.
A kind of preparation method of carbon-based photothermal conversion film, paper handkerchief is placed in inert protective gas and is carbonized, from room 20-25 degrees Celsius of temperature are warming up to 400-450 degrees Celsius with 1-5 degrees Celsius per minute of speed and keep the temperature 1-5h, then with every point 1-5 degrees Celsius of clock of speed is warming up to 800-850 degrees Celsius and keeps the temperature 1-5h, cools to room temperature 20-25 with the furnace after being carbonized Degree Celsius.
Preferably, 400-430 degrees Celsius are warming up to 1-3 degrees Celsius per minute of speed from 20-25 degrees Celsius of room temperature And 1-2h is kept the temperature, then be warming up to 800-820 degrees Celsius with 1-3 degrees Celsius per minute of speed and keep the temperature 1-2h, after being carbonized Cool to 20-25 degrees Celsius of room temperature with the furnace.
Specifically, using the preparation facilities equipment of carbon-based photothermal conversion film, casing knot is formed in view of inner and outer tubes Structure, so that paper handkerchief, which is completely immersed in always in inert protective gas atmosphere, carries out carbon by the way of being continuously passed through inert protective gas Change.Specific to the quartz ampoule in experiment, taking 3 centimetres of 30 cm diameter of length, May Flower tissue is wound on quartz ampoule (in i.e. Pipe) on, the both ends of quartz ampoule are supported with metallic support, then this entirety is put into tube furnace (tube furnace internal diameter 5.4cm), the quartz ampoule (i.e. outer tube) of tube furnace will constitute tube hub in a line with the quartz ampoule (i.e. inner tube) for being wound with tissue Two-layer pipe (i.e. coaxial sleeve structure), then tube furnace is sealed, and be passed through inert protective gas discharge air and oxygen After gas, heating is carbonized.
The preparation of carbon film can be realized according to technical solution of the present invention, carbon-base film photothermal conversion system of the invention has The performance of superior photic water evaporation.C film material is relatively light and is made of completely carbon fiber, stronger from floating capacity, can be with Spontaneous swims in water-air interface, contacts with the water surface sufficiently and effective.The result shows that this hydrophobicity photo-thermal film floating On the water surface, under the same conditions, the evaporation rate of water can be significantly improved.C film is due to the absorption with wide spectrum, photo-thermal The advantages that high conversion efficiency, simple processing synthesis, the preparation of optothermal material can be widely used in.
Detailed description of the invention
Fig. 1 is the appliance arrangement schematic diagram (1) that film preparation is carried out in the present invention, wherein 1 is outer tube, 2 be inner tube, and 3 are Heating device, 4 be support member, and 5 be paper handkerchief.
Fig. 2 is the appliance arrangement schematic diagram (2) that film preparation is carried out in the present invention, and 1 is outer tube, and 2 be inner tube, and 4 be support Component.
Fig. 3 is the X-ray diffraction spectrogram using the carbon-based photothermal conversion film of technical solution of the present invention preparation.
Fig. 4 is the Raman spectroscopy using the carbon-based photothermal conversion film of technical solution of the present invention preparation.
Fig. 5 is the power spectrum spectrogram using the carbon-based photothermal conversion film of technical solution of the present invention preparation.
Fig. 6 is the absorptance test chart using the carbon-based photothermal conversion film of technical solution of the present invention preparation.
Fig. 7 is the test of the reflectivity and transmitance using the carbon-based photothermal conversion film of technical solution of the present invention preparation Figure.
Fig. 8 is tested using the carbon-based photothermal conversion film of technical solution of the present invention preparation and the absorbance of raw material paper handkerchief Figure.
Fig. 9 is the SEM photograph using the carbon-based photothermal conversion film of technical solution of the present invention preparation.
Figure 10 is the SEM photograph of raw material paper handkerchief.
Figure 11 is the contact angle test using carbon-based the photothermal conversion film and raw material paper handkerchief of technical solution of the present invention preparation Figure, wherein a is carbon-based photothermal conversion film, and b is paper handkerchief.
Figure 12 is the photo-thermal test device setting schematic diagram that the present invention uses.
Figure 13 is the water quality quantitative change using the carbon-based photothermal conversion film of technical solution of the present invention preparation under different illumination Change test chart.
Figure 14 is water quality variation test chart of the hydrophobization paper handkerchief under different illumination as a comparison.
Figure 15 is water quality variation test chart of the blank control group under different illumination.
Figure 16 is the evaporation rate using the carbon-based photothermal conversion film of technical solution of the present invention preparation under different illumination Test chart.
Figure 17 is evaporation rate test chart of the hydrophobization paper handkerchief under different illumination as a comparison.
Figure 18 is the carbon-based photothermal conversion film using technical solution of the present invention preparation relative to hydrophobization as a comparison Raising factor test chart of paper handkerchief when one hour.
Specific embodiment
Technical solution of the present invention is further illustrated combined with specific embodiments below.The handkerchief of paper selection court cards in May Paper.
As shown in attached drawing 1-2, the appliance arrangement of film preparation, including inner and outer tubes are carried out, in inner tube outer surface and outside Support member is set between pipe internal surface, so that inner and outer tubes are coaxially disposed to form tube-in-tube structure, inner tube is arranged in paper handkerchief On outer surface.
Furtherly, both ends of the inner tube, paper handkerchief is arranged in outside the inner tube between two-end support parts for support member setting On surface, the quantity of paper handkerchief is at least 1, can be the overlay structure of multiple paper handkerchiefs.
Furtherly, support member is circumferentially uniformly distributed, and preferably 2-6.
Furtherly, support member is metallic support, and outer tube and inner tube select quartz ampoule.
Carry out in use, the appliance arrangement being made of inner and outer tubes is placed in heating device (i.e. tube furnace plus Thermal region).In view of inner and outer tubes formed cannula structure, by the way of being continuously passed through inert protective gas so that paper handkerchief always It is completely immersed in inert protective gas atmosphere and is carbonized.
Specific to the quartz ampoule in experiment, taking 3 centimetres of 30 cm diameter of length, May Flower tissue is wound on quartz ampoule In (i.e. inner tube), the both ends of quartz ampoule are supported with metallic support, then this entirety is put into tube furnace (tube furnace Internal diameter 5.4cm), the quartz ampoule (i.e. outer tube) of tube furnace and the quartz ampoule (i.e. inner tube) for being wound with tissue will constitute tube hub one The two-layer pipe (i.e. coaxial sleeve structure) risen, then tube furnace is sealed, and be passed through inert protective gas discharge air and After oxygen, heating is carbonized, and cools to room temperature with the furnace in inert protective gas atmosphere after being carbonized.
Embodiment 1
1. inert protective gas is argon gas
2. May Flower handkerchief paper size 10cm*5cm
3. being warming up to 400 degrees Celsius from 20 degrees Celsius of room temperature with 5 degrees Celsius of speed per minute and keeping the temperature 2h, so that handkerchief Paper solidification, then be warming up to 850 degrees Celsius with 5 degrees Celsius of speed per minute and keep the temperature 1h, so that tissue is carbonized, after being carbonized Cool to 20 degrees Celsius of room temperature with the furnace.
Embodiment 2
1. inert protective gas is nitrogen
2. May Flower handkerchief paper size 10cm*10cm
3. being warming up to 420 degrees Celsius from 25 degrees Celsius of room temperature with 1 degree Celsius of speed per minute and keeping the temperature 1h, so that handkerchief Paper solidification, then be warming up to 800 degrees Celsius with 1 degree Celsius of speed per minute and keep the temperature 5h, so that tissue is carbonized, after being carbonized Cool to 20 degrees Celsius of room temperature with the furnace.
Embodiment 3
1. inert protective gas is helium
2. May Flower handkerchief paper size 10cm*15cm
3. being warming up to 450 degrees Celsius from 22 degrees Celsius of room temperature with 3 degrees Celsius of speed per minute and keeping the temperature 5h, so that handkerchief Paper solidification, then be warming up to 840 degrees Celsius with 3 degrees Celsius of speed per minute and keep the temperature 2h, so that tissue is carbonized, after being carbonized Cool to 20 degrees Celsius of room temperature with the furnace.
Embodiment 4
1. inert protective gas is argon gas
2. May Flower handkerchief paper size 10cm*5cm, selects the overlay structure of 5 paper handkerchiefs
3. being warming up to 450 degrees Celsius from 25 degrees Celsius of room temperature with 5 degrees Celsius of speed per minute and keeping the temperature 3h, so that handkerchief Paper solidification, then be warming up to 820 degrees Celsius with 5 degrees Celsius of speed per minute and keep the temperature 5h, so that tissue is carbonized, after being carbonized Cool to 25 degrees Celsius of room temperature with the furnace.
Carbon film prepared by the present invention and raw material paper handkerchief are characterized, it is specific as shown in the picture.In Fig. 3, figure has Strong peak structure is 20 degree and 40 degree there are two bulge in the angle of diffraction, illustrates that synthesized material is not by completely by graphite Carbon composition, there are also non-graphitized carbon.It is the graphite tape of carbon material when the Raman shift of Raman spectrum is 1600 in Fig. 4,1360 When be imperfect tape it is corresponding be no graphited structure.As shown in Figure 5, the carbon element content of the material of preparation is 100%.Such as Shown in Fig. 6-8, the absorptance of carbon film is prepared 96% or so, reflectivity is approximately equal to 4%, and transmitance is approximately equal to 0% (absorptance =1- reflectivity-transmitance), absorbance has biggish promotion after paper handkerchief carbonization.As shown in attached drawing 9 and 10, it is respectively from a to f Enlarged drawing from low power to high power, it will be seen that carbon-based films are formed by distorting irregular carbon fiber, are existed between fiber and fiber More gap, this plays the role of the absorption of luminous energy and the generation of steam vital;The sample before and after carbonization Pattern is still and consists of fibers there is no particularly apparent variation.
As shown in figure 11, wellability test is done respectively to carbon-based photo-thermal film and paper handkerchief, discovery paper handkerchief in test is worked as in liquid Drop is just siphoned away from probe when just having contacted paper handkerchief surface, and paper handkerchief shows superpower water imbibition.And the paper handkerchief after being carbonized is worked as When water drop contact is to carbon film surface on probe, the certain apparent hydrophobic phenomenon contact angle shown is up to 140 degree or more, almost It is super-hydrophobic.
To carbon film of the present invention carry out photothermal conversion experiment, since carbon film use paper handkerchief for raw material, thus use raw material paper handkerchief into Row silicic acid anhydride obtains comparative example hydrophobization paper handkerchief, is cut into diameter in 3cm for paper handkerchief silicic acid anhydride-paper handkerchief as follows Disk, be placed on 100 milliliters of Shrek bottle, it is ensured that under ar gas environment, inject 50 μ L1H, 1H, 2H, 2H- Perfluorooctyltrichlorosilane (PFOTS) is into Shrek bottle.80 degrees Celsius, water-bath 30 minutes.1H,1H, 2H, 2H-perfluorooctyltrichlorosilane (PFOTS) are bought from J&K Scientific company.Such as Figure 12 institute Show, based on natural evaporation principle, using optical system, including solar simulator and its matching optics element, has carried out institute Some solar energy water purification experiments, the luminous intensity of solar simulator are easily controlled.By the power for adjusting solar simulator With the distance between evaporator and solar simulator, the intensity of light can control.Light power meter can be with the intensity of accurate recording light To evaporator.Water container insulating layer can also reduce water temperature loss.With the mass change of parsing balance real-time detection water.300W xenon Lamp (cel-hxuv300) comes that solar simulating radiation, that bore is adjusted to evaporator is identical using 1.5 filter.By New Port 91150v light power meter measures intensity of illumination, such as 1 times of sun (exposure intensity), 2 times of sun (exposure intensity), the 3 times of sun (irradiations Intensity).The solar energy of simulation shines directly on evaporator (carbon film on the water surface is arranged in).In certain time interval Interior, the weight of the water in container is recorded.
As shown in attached drawing 13-15, the carbon film of the invention evaporation capacity of one hour water in one times of Intensity of the sunlight reaches To 0.82 kilograms per square meter, two times of whens are 1.83, and whens three times is 3.54;Hydrophobization paper handkerchief is in one times of Intensity of the sunlight one Hour the evaporation capacity of water reach 0.41 kilograms per square meter, two times of whens are 0.80, and whens three times is 1.28;Blank group, i.e., directly Water surface situation is irradiated, in one times of Intensity of the sunlight, the evaporation capacity of one hour water reaches 0.41 kilograms per square meter, and two times When be 0.80, whens three times is 1.62.As shown in attached drawing 16-17, carbon film of the invention is in one times of Intensity of the sunlight one hour When the evaporation rate of water reach 1.01 kilograms per square meters per hour, two times of whens are 2.33, and whens three times is 4.45;It is hydrophobic The evaporation rate of water when changing paper handkerchief in one times of Intensity of the sunlight one hour reaches 0.54 kilograms per square meter per small When, two times of whens are 1.93 when being 1.18 three times.As shown in figure 18, the factor=carbon film evaporation rate/paper membrane evaporation speed is improved Rate, under identical intensity of illumination, carbon film of the present invention is better than hydrophobization paper handkerchief to the facilitation of evaporation, in the three times sun, improves The factor is up to 2.36.It follows that under the same conditions, although being all hydrophobic performance, carbon film of the invention is shown more preferably Photothermal conversion performance, that is, be better able to promote water evaporation.
Content carries out the adjustment of technological parameter according to the present invention, and the preparation of carbon film can be achieved and show and embodiment base This consistent performance.Illustrative description is done to the present invention above, it should which explanation is not departing from core of the invention In the case of, any simple deformation, modification or other skilled in the art can not spend being equal for creative work to replace It changes and each falls within protection scope of the present invention.

Claims (10)

1. a kind of preparation method of carbon-based photothermal conversion film, which is characterized in that paper handkerchief is placed in inert protective gas and is carried out Carbonization is warming up to 400-450 degrees Celsius from 20-25 degrees Celsius of room temperature with 1-5 degrees Celsius per minute of speed and keeps the temperature 1- 5h, then be warming up to 800-850 degrees Celsius with 1-5 degrees Celsius per minute of speed and keep the temperature 1-5h, the furnace cooling after being carbonized To 20-25 degrees Celsius of room temperature.
2. a kind of preparation method of carbon-based photothermal conversion film according to claim 1, which is characterized in that from room temperature 20- 25 degrees Celsius are warming up to 400-430 degrees Celsius with 1-3 degrees Celsius per minute of speed and keep the temperature 1-2h, then with 1-3 per minute Degree Celsius speed be warming up to 800-820 degrees Celsius and keep the temperature 1-2h, it is Celsius to cool to room temperature 20-25 with the furnace after being carbonized Degree.
3. a kind of preparation method of carbon-based photothermal conversion film according to claim 1 or 2, which is characterized in that use Continuously the mode of inert protective gas is passed through so that paper handkerchief is completely immersed in always in inert protective gas atmosphere is carbonized.
4. a kind of preparation method of carbon-based photothermal conversion film according to claim 3, which is characterized in that use carbon-based light Support is arranged in the preparation facilities equipment of thermal transition film, including inner and outer tubes between inner tube outer surface and outer pipe internal surface Component, so that inner and outer tubes are coaxially disposed to form tube-in-tube structure, paper handkerchief is arranged on the outer surface of inner tube.
5. a kind of preparation method of carbon-based photothermal conversion film according to claim 4, which is characterized in that support member is set It sets both ends of the inner tube, paper handkerchief is arranged on the inner tube outer surface between two-end support parts.
6. a kind of preparation method of carbon-based photothermal conversion film according to claim 4, which is characterized in that support member edge Circumferencial direction be uniformly distributed, preferably 2-6.
7. a kind of preparation method of carbon-based photothermal conversion film according to claim 4, which is characterized in that support member is Metallic support, outer tube and inner tube select quartz ampoule.
8. the preparation facilities of carbon-based photothermal conversion film, which is characterized in that including inner and outer tubes, in inner tube outer surface and outer tube Support member is set between inner surface, so that inner and outer tubes are coaxially disposed to form tube-in-tube structure, the outer of inner tube is arranged in paper handkerchief On surface.
9. the preparation facilities of carbon-based photothermal conversion film according to claim 8, which is characterized in that support member setting exists The both ends of inner tube, paper handkerchief are arranged on the inner tube outer surface between two-end support parts.
10. the preparation facilities of carbon-based photothermal conversion film according to claim 8, which is characterized in that support member along Circumferencial direction is uniformly distributed, and preferably 2-6;Support member is metallic support, and outer tube and inner tube select quartz ampoule.
CN201810202023.9A 2018-03-12 2018-03-12 A kind of preparation method of carbon-based photothermal conversion film Pending CN110255523A (en)

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Application publication date: 20190920