CN106637921B - A kind of polyacrylonitrile/copper sulfide photo-thermal nano-fiber cloth and its preparation and application - Google Patents
A kind of polyacrylonitrile/copper sulfide photo-thermal nano-fiber cloth and its preparation and application Download PDFInfo
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- CN106637921B CN106637921B CN201610874865.XA CN201610874865A CN106637921B CN 106637921 B CN106637921 B CN 106637921B CN 201610874865 A CN201610874865 A CN 201610874865A CN 106637921 B CN106637921 B CN 106637921B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/55—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
- D06M11/56—Sulfates or thiosulfates other than of elements of Groups 3 or 13 of the Periodic System
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
Abstract
The present invention relates to a kind of polyacrylonitrile/copper sulfide photo-thermal nano-fiber cloth and its preparations and application, and using polyacrylonitrile (PAN) nanofiber as matrix, copper sulfide CuS nano particle is distributed in polyacrylonitrile (PAN) nanofiber surface.Preparation: by containing mantoquita PAN nano-fiber cloth immerse sulphur source solution in, carry out vulcanizing treatment, drying to get.The present invention extends to optothermal material on solid fabric from solution, breaches the limitation that optothermal material uses, and is expected to be widely used in the fields such as solar heating equipment of new generation and solar energy warm clothes of new generation.
Description
Technical field
The invention belongs to photo-thermal nano material and its preparation and application field, in particular to a kind of polyacrylonitrile/copper sulfide
Photo-thermal nano-fiber cloth and its preparation and application.
Background technique
Optothermal material is a kind of emerging function nano material that the luminous energy of specific band can be converted to directly to thermal energy.Mesh
Before, optothermal material is mainly used as a kind of Cancer therapeutic agents, be widely studied (Adv.Mater.2011,23,3542-
3547；Adv.Mater.2013,25:2095-2100；Adv.Mater.2016,28:245-253.).Current optothermal material master
There are four major class: organic nano material, metal-based nano material, c-based nanomaterial, semiconductor nano material.Wherein, it partly leads
Body photo-thermal nano material is a kind of photo-thermal material, have many advantages, such as to prepare it is simple, cheap, be easy to functionalization.As
A kind of medical treatment reagent, optothermal material usually need to be dispersed in water or biomass solution, this makes people for photo-thermal
The research and application of material only reside in the solution of photo-thermal nano material, limit its scope of application.
Luminous energy can be converted into thermal energy by optothermal material, if the heat generated can be used directly in real life
It warms oneself, this will have huge potential value for solar heating equipment of new generation.However, photo-thermal material in the solution
The attainable temperature of material institute is limited, and heating rate is simultaneously unhappy, and generated heat is limited in solution, uses in daily life
It is inconvenient, it is difficult to be popularized and be widely applied.Therefore, it in order to expand the application range of optothermal material, needs optothermal material
It is combined with the basis material of other forms, for example prepares photothermal conversion cloth, this can be by the photothermal conversion property of material from molten
Liquid status is extended on solid matrix, so that the use scope of optothermal material greatly increases, for optothermal material in daily life
In use and promote, be of great significance.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of polyacrylonitrile/copper sulfide photo-thermal nano-fiber cloth and its systems
It is standby and application, synthetic method of the present invention is simple, and synthesis condition is mild, it is cheap and have very wide light abstraction width, this hair
It is bright by the way that copper sulfide nano material and polymers for general use nanofiber is mutually compound, preparing can be efficiently direct by sunlight
It is self-produced to can be used for heating of house, dual-use camping outdoors facility, new type solar energy for the photo-thermal nano-fiber cloth for being converted to thermal energy
The energy consumed by warming is saved in the fields such as hot warmth-retaining clothing, is improved amenity, is set in solar heating of new generation
There is larger application prospect in applying.
A kind of polyacrylonitrile of the invention/copper sulfide photo-thermal nano-fiber cloth, the photo-thermal nano-fiber cloth is with polypropylene
Nitrile PAN nanofiber is matrix, and copper sulfide CuS nano particle is distributed in polyacrylonitrile (PAN) nanofiber surface.
A kind of polyacrylonitrile of the invention/copper sulfide photo-thermal nano-fiber cloth preparation method, comprising:
(1) polyacrylonitrile (PAN) is added in organic solvent, stirring and dissolving obtains PAN solution, mantoquita is then added, obtains
Then electrostatic spinning raw material solution carries out electrostatic spinning, obtain the PAN nano-fiber cloth containing mantoquita；
(2) the PAN nano-fiber cloth by above-mentioned containing mantoquita immerses in sulphur source solution, carries out vulcanizing treatment, cold at room temperature
But drying is taken out afterwards, obtains polyacrylonitrile/copper sulfide photo-thermal nano-fiber cloth.
The average molecular weight of polyacrylonitrile (PAN) is 150000 in the step (1)；Organic solvent is N, N- dimethyl formyl
Amine DMF.
The mass percentage concentration of PAN is 5~12% in PAN solution in the step (1).
Under the conditions of stirring solvent is 60 DEG C in the step (1), it is stirred overnight dissolution.
Mantoquita is copper sulphate, copper chloride, copper nitrate, copper acetate and acetylacetone copper Cu (C in the step (1)5H7O2)2
One or more of, copper ion concentration is 0.1~0.8mol/L in electrostatic spinning raw material solution.
Electrostatic spinning process parameter in the step (1) are as follows: 10~25kV of voltage, 20~200 μ L/ of solution fltting speed
Min, 10~50 DEG C of spinning temperature, envionmental humidity 20~60%, receiving distance is 15~30cm, and aluminium foil collects Nanowire
Dimension.
The average diameter of the PAN nanofiber containing mantoquita is 200~1000nm in the step (1), with a thickness of 40~
1500μm。
Sulphur source is one or more of ammonium sulfide, vulcanized sodium, thiocarbamide, carbon disulfide and elemental sulfur in the step (2),
The solvent of copper source solution is one or more of water, ethyl alcohol, carbon disulfide, in sulphur source solution the concentration of element sulphur be 0.01~
0.5mol/L。
Vulcanizing treatment in the step (2) are as follows: curing temperature is 50~100 DEG C, and vulcanization time is 0.5~6h.
A kind of polyacrylonitrile of the invention/copper sulfide photo-thermal nano-fiber cloth application, in solar energy warm equipment and too
Application in positive energy insulation garment.
Invention of the present invention has obtained PAN-CuS photo-thermal nano-fiber cloth using two-step method under conditions of more mild, has
There are very wide absorbing properties and efficient photothermal conversion performance.Relative to the thermal energy that CuS under solution state is generated, photo-thermal nanometer
Heat caused by fiber cloth is used directly in daily heating, is protected in solar heating equipment of new generation and solar energy of new generation
Warmly taking in dress has huge application value.
The present invention uses two-step method, and the PAN nano fiber non-woven fabric of copper source presoma is first had using electrostatic spinning preparation,
It carries out again In-situ sulphiding, obtains PAN-CuS photo-thermal nano-fiber cloth.In the present invention, PAN nanofiber provides light as matrix
The carrier function of hot material, CuS provide good photo absorption performance and photothermal conversion performance as functional materials.
Photo-thermal nano-fiber cloth in the present invention has very wide light abstraction width (200~2000nm) and efficient light
Hot-cast socket ability can absorb most of luminous energy in sunlight, and be converted directly into thermal energy, under xenon lamp irradiation, surface temperature
Degree can increase rapidly and more than 100 DEG C.
Beneficial effect
(1) present invention is prepared for a kind of photo-thermal nanofiber using simple synthetic method under mild synthesis condition
Cloth, it is cheap, there is very wide photo absorption performance and efficient photothermal conversion performance；
(2) CuS nanoparticles optothermal material is extended in fibrous material by the present invention from solution for the first time, breaches solution state
The use of lower optothermal material is limited to, so that heat caused by optothermal material can be directly used for warming, can save the winter
The energy consumption that season heating generates, possesses huge answer in solar heating equipment of new generation, new type solar energy insulation garment
With value.
Detailed description of the invention
Fig. 1 is prepared PAN-Cu (C in the embodiment of the present invention 15H7O2)2Low power (a), the high power (b) of nano-fiber cloth
SEM picture；
Fig. 2 is (a) low power of prepared PAN-CuS photo-thermal nano-fiber cloth in the embodiment of the present invention 1, (b) high power SEM figure
Piece, and (c) low power and (d) high-resolution TEM photo；
Fig. 3 is prepared PAN-CuS photo-thermal nano-fiber cloth and pure PAN nano-fiber cloth in the embodiment of the present invention 1
XRD spectrum；
Fig. 4 is prepared PAN-CuS, PAN-Cu (C in the embodiment of the present invention 15H7O2)2With the suction of pure PAN nano-fiber cloth
Light spectrum；
Fig. 5 is prepared PAN-CuS, PAN-Cu (C in the embodiment of the present invention 15H7O2)2With pure PAN nano-fiber cloth flat
Equal light intensity 2.1W/cm2Under heating map；
Fig. 6 is the extinction spectrum of prepared PAN-CuS nano-fiber cloth in the embodiment of the present invention 2；
Fig. 7 is prepared PAN-CuS nano-fiber cloth in the embodiment of the present invention 2 in average intensity 2.1W/cm2Under heating
Map.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
2.1g polyacrylonitrile is weighed with assay balance, is added in the round-bottomed flask equipped with 30ml organic solvent DMF, is put into and adds
In hot jacket, temperature setting is 60 DEG C, magnetic stirrer over night dissolution.Second day, the Cu of 0.2658g is added in gained PAN solution
(C5H7O2)2, de-soak is stood after being uniformly dissolved, obtains opaque bluish violet spinning solution.10mL spinning solution is taken to be put into injection
Electrostatic spinning is carried out in device, sets spinning temperature as 50 DEG C, spinning voltage 16.91kV, and injecting speed is 45 μ L/min, relatively
Humidity is 25% or so, is collected nanofiber using aluminium foil, and receiving distance is 20cm, obtains the PAN nanofiber of cupric
Cloth, from figure 1 it appears that the diameter distribution of these nanofibers is more uniform, average diameter is between 300~350nm.
It weighs 0.5404g Sodium Sulphate Nine Hydroxide to be added in 45mL deionized water, the vulcanized sodium for being configured to 0.05mol/L is molten
Liquid takes the PAN-Cu (C of 9 × 15cm5H7O2)2Nano-fiber cloth immerses in the sodium sulfide solution matched together together with aluminium foil,
It is put it into 80 DEG C of baking oven later, the setting time is 120 minutes, after its natural cooling, takes out sample in 60 DEG C of baking ovens
Obtaining PAN-CuS photo-thermal nano-fiber cloth after middle drying, the pattern of the nanofiber is as shown in Fig. 2, as seen from the figure, and CuS nanometers
Crystal is evenly distributed PAN nanofiber surface by growth in situ, by TEM photo (Fig. 2 c), can more clearly observe
To the CuS nano particle of PAN nanofiber and its surface, high-resolution TEM photo shows CuS nano particle height crystallization, lattice
It is spaced about 0.32nm (see Fig. 2 d), the compound JCPDS 06-0464 of the diffraction maximum in XRD spectrum has further proved CuS's
Crystallinity.Fig. 4 is pure PAN nanofiber, PAN-Cu (C5H7O2)2The suction of nano-fiber cloth and PAN-CuS photo-thermal nano-fiber cloth
Light spectrum, as seen from the figure, PAN-CuS photo-thermal nano-fiber cloth have light absorptive in the range of from 200nm to 2000nm, cover
The overwhelming majority in solar spectrum is 2.1W/cm in average intensity2Xenon lamp simulator under, PAN-CuS photo-thermal nano-fiber cloth
It can be brought rapidly up, 3 minutes internal surface temperatures can reach 101 DEG C (Fig. 5).
Embodiment 2
1.4g polyacrylonitrile is weighed with assay balance, is added in the round-bottomed flask equipped with 20ml organic solvent DMF, is put into and adds
In hot jacket, temperature setting is 60 DEG C, magnetic stirrer over night dissolution.Second day, the Cu of 0.1329g is added in gained PAN solution
(C5H7O2)2, de-soak is stood after being uniformly dissolved, obtains opaque bluish violet spinning solution.20mL spinning solution is taken to be put into injection
Electrostatic spinning is carried out in device, sets spinning temperature as 35 DEG C, spinning voltage 16.08kV, and injecting speed is 35 μ L/min, relatively
Humidity is 25% or so, is collected nanofiber using aluminium foil, and receiving distance is 15cm, obtains the PAN nanofiber of cupric
Cloth.
0.9ml ammonium sulfide solution (element sulphur mass percent >=8%) is measured with liquid-transfering gun to be added in 45mL deionized water,
It is configured to the sodium sulfide solution of 0.05mol/L, takes the PAN-Cu (C of 9 × 15cm5H7O2)2Nano-fiber cloth, together together with aluminium foil
It immerses in the sodium sulfide solution matched, is put it into 80 DEG C of baking oven later, the setting time is 120 minutes, to its nature
After cooling, takes out after sample is dried in 60 DEG C of baking ovens and obtain PAN-CuS photo-thermal nano-fiber cloth.Fig. 6 is using under this condition
The extinction spectrum of obtained PAN-CuS photo-thermal nano-fiber cloth, as seen from the figure, PAN-CuS photo-thermal nano-fiber cloth is in broadband
It is interior that there is stronger light absorptive, cover the overwhelming majority in solar spectrum, is 2.1W/cm in average intensity2Xenon lamp simulator shine
It penetrates down, PAN-CuS photo-thermal nano-fiber cloth can be brought rapidly up, and 3 minutes internal surface temperature highests can be more than 85 DEG C (Fig. 7).
Claims (8)
1. a kind of polyacrylonitrile/copper sulfide photo-thermal nano-fiber cloth, it is characterised in that: the photo-thermal nano-fiber cloth is with polypropylene
Nitrile PAN nanofiber is matrix, and copper sulfide CuS nano particle is distributed in polyacrylonitrile (PAN) nanofiber surface；Wherein photo-thermal is received
Rice fiber cloth is prepared by following method:
(1) polyacrylonitrile (PAN) is added in organic solvent, stirring and dissolving obtains PAN solution, mantoquita is then added, obtains electrostatic
Then spinning solution carries out electrostatic spinning, obtain the PAN nano-fiber cloth containing mantoquita；Wherein mantoquita is acetylacetone copper Cu
(C5H7O2)2；
(2) the PAN nano-fiber cloth by above-mentioned containing mantoquita immerses in sulphur source solution, carries out vulcanizing treatment, and drying obtains poly- third
Alkene nitrile/copper sulfide photo-thermal nano-fiber cloth；Wherein curing temperature is 50~100 DEG C, and vulcanization time is 0.5~6h.
2. a kind of polyacrylonitrile as described in claim 1/copper sulfide photo-thermal nano-fiber cloth preparation method, comprising:
(1) polyacrylonitrile (PAN) is added in organic solvent, stirring and dissolving obtains PAN solution, mantoquita is then added, obtains electrostatic
Then spinning solution carries out electrostatic spinning, obtain the PAN nano-fiber cloth containing mantoquita；Wherein mantoquita is acetylacetone copper Cu
(C5H7O2)2；
(2) the PAN nano-fiber cloth by above-mentioned containing mantoquita immerses in sulphur source solution, carries out vulcanizing treatment, and drying obtains poly- third
Alkene nitrile/copper sulfide photo-thermal nano-fiber cloth；Curing temperature is 50~100 DEG C, and vulcanization time is 0.5~6h.
3. a kind of polyacrylonitrile according to claim 2/copper sulfide photo-thermal nano-fiber cloth preparation method, feature exist
In: the average molecular weight of polyacrylonitrile (PAN) is 150000 in the step (1)；Organic solvent is N,N-dimethylformamide
DMF。
4. a kind of polyacrylonitrile according to claim 2/copper sulfide photo-thermal nano-fiber cloth preparation method, feature exist
In: the mass percentage concentration of PAN is 5~12% in PAN solution in the step (1).
5. a kind of polyacrylonitrile according to claim 2/copper sulfide photo-thermal nano-fiber cloth preparation method, feature exist
In: under the conditions of stirring solvent is 60 DEG C in the step (1), it is stirred overnight dissolution.
6. a kind of polyacrylonitrile according to claim 2/copper sulfide photo-thermal nano-fiber cloth preparation method, feature exist
In: copper ion concentration is 0.1~0.8mol/L in electrostatic spinning raw material solution in the step (1).
7. a kind of polyacrylonitrile according to claim 2/copper sulfide photo-thermal nano-fiber cloth preparation method, feature exist
In: electrostatic spinning process parameter in the step (1) are as follows: 10~25kV of voltage, 20~200 μ L/min of solution fltting speed are spun
10~50 DEG C of temperature of silk, envionmental humidity 20~60%, receiving distance is 15~30cm, and aluminium foil collects nanofiber.
8. a kind of polyacrylonitrile according to claim 2/copper sulfide photo-thermal nano-fiber cloth preparation method, feature exist
In: sulphur source is one or more of ammonium sulfide, vulcanized sodium, thiocarbamide, carbon disulfide and elemental sulfur, sulphur source in the step (2)
The concentration of solution is 0.01~0.5mol/L.
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| CN107235591B (en) * | 2017-06-28 | 2020-07-24 | 中国科学院合肥物质科学研究院 | Application of photo-thermal conversion copper sulfide composite film in water treatment |
| CN107675275B (en) * | 2017-11-17 | 2020-11-03 | 苏州大学 | Two-dimensional ultrathin material and preparation method thereof |
| CN109888219A (en) * | 2019-02-22 | 2019-06-14 | 东华大学 | A kind of Cu oxide/carbon nano-fiber/sulfur electrode material and its preparation and application |
| CN110195351B (en) * | 2019-06-20 | 2021-10-19 | 中原工学院 | Preparation method of carbon nanotube/copper sulfide composite electromagnetic shielding fabric |
| CN110341257A (en) * | 2019-07-26 | 2019-10-18 | 南通大学 | A kind of multi-functional compound coat fabric and preparation method thereof |
| CN111074539B (en) * | 2019-12-27 | 2022-04-12 | 武汉纺织大学 | Fabric with core-shell structure photothermal conversion material and preparation method thereof |
| CN112599777B (en) * | 2020-12-14 | 2022-09-27 | 河北工业大学 | Preparation method and application of transition metal sulfide/nitrogen and sulfur co-doped carbon composite fiber electrode material |
| CN112853511A (en) * | 2020-12-31 | 2021-05-28 | 南京工业大学 | Method for preparing photo-thermal fiber by microfluid air jet spinning |
| CN112899887A (en) * | 2021-01-19 | 2021-06-04 | 中国科学院合肥物质科学研究院 | Temperature-adjusting anti-fouling fiber membrane and temperature-adjusting anti-fouling breathable double-layer fiber membrane based on same |
| CN113680216A (en) * | 2021-09-05 | 2021-11-23 | 河海大学 | Preparation method of photo-thermal distillation membrane with catalytic function |
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