CN108625155B - Preparation method of fiber for generating photocurrent by using sunlight - Google Patents

Preparation method of fiber for generating photocurrent by using sunlight Download PDF

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CN108625155B
CN108625155B CN201810235669.7A CN201810235669A CN108625155B CN 108625155 B CN108625155 B CN 108625155B CN 201810235669 A CN201810235669 A CN 201810235669A CN 108625155 B CN108625155 B CN 108625155B
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deionized water
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pet
fiber
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CN108625155A (en
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彭志勤
李晓涵
万军民
胡智文
王秉
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Zhejiang University of Technology ZJUT
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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
    • D06M11/32—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic System; Titanates; Zirconates; Stannates; Plumbates
    • 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
    • D06M11/83—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 metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
    • 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
    • D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
    • 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
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
    • 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
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy

Abstract

The invention discloses a preparation method of a fiber for generating photocurrent by sunlight, which comprises the following preparation steps: selecting PET fibers with smooth surfaces, and carrying out oil removal, coarsening, sensitization and activation on the PET fibers; preparing chemical copper plating solution, putting the PET fiber into the copper plating solution to plate the PET fiber with copper; preparing a titanium dioxide nanotube by a hydrothermal method; adopting a condensation reflux method to compound protoporphyrin and titanium dioxide nanotubes to obtain H2TCPP-TNT solid powder; h is to be2The TCPP-TNT binary compound is smeared on copper-plated PET fiber, then a layer of silicon rubber is smeared, and the silicon rubber is solidified in an oven.

Description

Preparation method of fiber for generating photocurrent by using sunlight
Technical Field
The present invention relates to a method for preparing a fiber, and more particularly, to a method for preparing a fiber using sunlight to generate photocurrent.
Background
Porphyrin is a photosensitizer, can produce photoelectron under the irradiation of sunlight, and can inject the photoelectron into the conduction band of semiconductor, the titanium dioxide nanotube is an ideal semiconductor, can transfer the electron into the conductive base material, and can make the conductive base material produce current, and the PET fibre is a chemical fibre with extensive application, and its production cost is very low, and has good breaking and stretching properties, and the fibre is long-thread-like, and the PET can be made into very thin fibre, and its flexibility is good. According to the invention, a layer of copper is plated on the PET fiber by using a chemical copper plating method, so that the PET fiber has better conductivity, the PET fiber after copper plating is used as a conductive base material, a binary compound of protoporphyrin and titanium dioxide nanotubes is coated on the PET fiber, the PET fiber is coated by using transparent silicon rubber, and the silicon rubber is cured to obtain the composite fiber.
Disclosure of Invention
The invention aims to provide a preparation method of a fiber for generating photocurrent by using sunlight, which has the technical characteristics of good flexibility, low cost, photocurrent generated after light irradiation and the like.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the invention relates to a preparation method of a fiber for generating photocurrent by sunlight, which comprises the following preparation steps:
step 1): adding PET fiber with smooth surface into sodium hydroxide solution with concentration of 0.1-0.15mol/L, and placing at water bath temperature of 60-70 deg.C for 3-5 min;
step 2): adding 7-8g of KMnO4 solid particles into 500ml of deionized water, stirring to dissolve, and adding 18-22ml of 98% H2SO4Magnetically stirring for 10-15min to form uniform roughening solution, immersing the deoiled PET fiber in the roughening solution at 35-45 ℃ for 4-6min, taking out the PET fiber, putting the PET fiber into oxalic acid solution with the concentration of 12g/L, placing the solution at the water bath temperature of 30-40 ℃ for 3-5min, and then washing the solution for 1-2 times by using deionized water;
step 3): adding 4-6g SnCl into 500ml deionized water2Adding 18-22ml of HCl with the concentration of 38% into the solid particles, stirring and dissolving to form uniform sensitizing solution, immersing the PET fibers treated in the step 2) into the sensitizing solution, and placing the PET fibers at the water bath temperature of 35-45 ℃ for 4-6 min;
step 4): adding 0.08-0.1g of PdCl into 200ml of deionized water2Stirring and dissolving solid powder and 3-4ml of HCl with the concentration of 38% to form uniform activation liquid, immersing the PET fibers treated in the step 3) in the activation liquid, and placing the PET fibers at the water bath temperature of 35-45 ℃ for 4-6 min;
step 5): 8-12g of the mixture was dissolved in 160ml of 140-160ml of deionized waterCuSO4Dissolving 0.9-1.1g of NiSO in 40-50ml of deionized water4·6H2O, dissolving 42-48g of sodium tartrate in 160ml of 140-160ml of deionized water, dissolving 6.5-7.5g of NaOH in 40-50ml of deionized water, sequentially pouring the CuSO4 solution, the NiSO4 solution, the sodium tartrate solution and the NaOH solution into a 500ml volumetric flask, then adding 7-8ml of HCHO, and finally adding deionized water to 500ml to obtain electroless copper plating solution, putting the PET fibers treated in the step 4) into the copper plating solution, and placing the PET fibers at the water bath temperature of 33-37 ℃ for 25-35 min;
step 6): weighing 5.5-6.5g of nano titanium dioxide powder, dispersing the nano titanium dioxide powder in 155ml of NaOH solution, fully stirring the solution, pouring the solution into a reaction kettle, placing the reaction kettle in an oven with the temperature of 130-140 ℃ for reaction for 36h, placing the reaction kettle in a centrifuge with the rotating speed of 3000r/s for centrifugation to obtain a white precipitate, washing the white precipitate by using a solution with the concentration of 0.1-0.2mol/LHCl until the PH is 1.5, stirring the solution at normal temperature for 24-25h, performing ultrasonic treatment for 1.5h, placing the solution in the centrifuge with the rotating speed of 3000r/s to obtain the white precipitate again, washing the white precipitate to be neutral by using deionized water, and placing the precipitate in the oven with the temperature of 70-80 ℃ for drying to obtain a titanium dioxide;
step 7): preparation H2TCPP-TNT binary complex: weighing 15-20mg protoporphyrin, dissolving in 100ml N 'N-dimethylformamide, adding 0.8-1.0g titanium dioxide nanotube obtained in the step 6), stirring fully to obtain a mixed solution, pouring the mixed solution into a 250ml single-neck flask, heating to 120 ℃ in dark environment, reacting for 5-6H, vacuum filtering to obtain a precipitate, washing with 15-25ml N' N-dimethylformamide, washing with deionized water for 2-3min, and finally drying in a 60-70 ℃ oven to obtain H2TCPP-TNT powder;
step 8): laying a layer of H with the thickness of 1-2mm on clean and smooth white paper2TCPP-TNT powder, laying the PET fiber obtained in the step 5) on the powder, and then scattering a layer of H on the PET fiber2TCPP-TNT powder, coating silicon rubber on PET fiber, placing in an oven at the temperature of 100-110 ℃ for baking for 30-40min, and curing the silicon rubber to obtain the composite fiber capable of generating current under the irradiation of sunlight, wherein the silicon rubber comprises a main agent and a curing agent, and the mass ratio of the main agent to the curing agent is 3-3.5: 1.
The invention relates to a preparation method of a fiber for generating photocurrent by sunlight, which comprises the following preparation steps:
step 1): adding PET fiber with smooth surface into sodium hydroxide solution with concentration of 0.12mol/L, and placing at water bath temperature of 65 ℃ for 4 min;
step 2): to 500ml of deionized water, 7.5g of KMnO4 solid particles were added, dissolved with stirring, and 20ml of 98% H was added2SO4Magnetically stirring for 12min to form uniform roughening solution, immersing the deoiled PET fiber in the roughening solution at 40 ℃ for 5min, taking out the PET fiber, putting the PET fiber into oxalic acid solution with the concentration of 12g/L, placing the PET fiber at the water bath temperature of 35 ℃ for 4min, and then washing the PET fiber for 1 time by using deionized water;
step 3): 5g of SnCl was added to 500ml of deionized water2Adding 20ml of HCl with the concentration of 38% into the solid particles, stirring and dissolving to form uniform sensitizing solution, immersing the PET fibers treated in the step 2) into the sensitizing solution, and placing the PET fibers at the water bath temperature of 40 ℃ for 4.5 min;
step 4): to 200ml of deionized water, 0.09g of PdCl was added2Stirring and dissolving solid powder and 3.5ml of HCl with the concentration of 38% to form uniform activation liquid, immersing the PET fibers treated in the step 3) in the activation liquid, and placing the PET fibers at the water bath temperature of 40 ℃ for 5 min;
step 5): dissolve 10g of CuSO in 150ml of deionized water4Dissolving 1.0g of NiSO in 45ml of deionized water4·6H2O, dissolving 45g of sodium tartrate in 150ml of deionized water, dissolving 8g of NaOH in 45ml of deionized water, and adding the above CuSO4Solution, NiSO4Sequentially pouring the solution, the sodium tartrate solution and the NaOH solution into a 500ml volumetric flask, then adding 7.5ml of HCHO, and finally adding deionized water to 500ml to obtain a chemical copper plating solution, putting the PET fibers treated in the step 4) into the copper plating solution, and placing the PET fibers at the water bath temperature of 35 ℃ for 30 min;
step 6): weighing 6g of nano titanium dioxide powder, dispersing the nano titanium dioxide powder in 150ml of NaOH solution, fully stirring the solution, pouring the solution into a reaction kettle, placing the reaction kettle in a 135 ℃ drying oven for reacting for 36 hours, placing the reaction kettle in a 3000r/s centrifugal machine for centrifuging to obtain a white precipitate, washing the white precipitate by using a 0.15mol/LHCl solution until the pH value is 1.5, stirring the solution for 24.5 hours at normal temperature, ultrasonically treating the solution for 1.5 hours, placing the solution in a 3000r/s centrifugal machine for obtaining the white precipitate again, washing the white precipitate to be neutral by using deionized water, and placing the precipitate in a 75 ℃ drying oven for drying to obtain a titanium dioxide nanotube;
step 7): preparation H2TCPP-TNT binary complex: weighing 17mg protoporphyrin, dissolving in 100ml N 'N-dimethylformamide, adding 0.9g titanium dioxide nanotube obtained in the step 6), fully stirring to obtain a mixed solution, pouring the mixed solution into a 250ml single-neck flask, heating to 120 ℃ in dark environment, reacting for 5.5H, vacuum-filtering to obtain a precipitate, washing with 20ml N' N-dimethylformamide, washing with deionized water for 2.5min, and finally drying in a 65 ℃ oven to obtain H2TCPP-TNT powder;
step 8): laying a layer of H with the thickness of 1.5mm on clean and smooth white paper2Placing the PET fiber obtained in the step 5) on the TCPP-TNT powder, spreading a layer of H2TCPP-TNT powder on the PET fiber, coating silicon rubber on the PET fiber, placing the PET fiber in an oven at 105 ℃ for drying for 35min, and curing the silicon rubber to obtain the composite fiber capable of generating current under the irradiation of sunlight, wherein the silicon rubber comprises a main agent and a curing agent, and the mass ratio of the main agent to the curing agent is 3: 1.
Compared with the prior art, the invention has the beneficial effects that:
1) the PET fibers are plated with copper in a chemical mode, operation is simple and convenient, the experimental process is short, and the insulated PET fibers can be changed into fibers with good conductivity. And before copper plating of the fibers, 0.5g/l PdCl is used2The acid solution activates the fiber, so that copper can be effectively plated on the fiber, and the copper plating effect is good;
2) using CuSO4、NiSO4·6H2Preparing copper plating solution by using O, sodium tartrate, NaOH and HCHO, separately dissolving solid medicines in the copper plating solution and then mixing the solid medicines to obtain uniform and precipitate-free copper plating solution, so that each part can be uniformly plated with a copper layer when the fiber is immersed in the copper plating solution;
3) by condensing the refluxThe method compounds the titanium dioxide nanotube and the protoporphyrin (the dosage ratio of the titanium dioxide nanotube to the protoporphyrin is 50-56.7:1), the time is only 5-6H, the process is short, and H can be successfully prepared2TCPP-TNT binary complex;
4) is coated with H by using silicone rubber2Wrapping TCPP-TNT powder with PET fiber to obtain H2The TCPP-TNT is firmly loaded on the PET fibers, and the silicon rubber is transparent, so that sunlight can shine on the photosensitizer through the silicon rubber;
5) the PET fiber is used as a conductive base material, and the composite fiber has good flexibility and low cost.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the embodiments of the present invention are not limited to the following examples.
Example 1
The invention relates to a preparation method of a fiber for generating photocurrent by sunlight, which comprises the following preparation steps:
step 1): adding PET fibers with smooth surfaces into a sodium hydroxide solution with the concentration of 0.1mol/L, and placing the PET fibers at the water bath temperature of 60 ℃ for 3 min;
step 2): to 500ml of deionized water, 7g of KMnO4 solid particles were added, dissolved with stirring, and 18ml of 98% H was added2SO4Magnetically stirring for 10min to form uniform roughening solution, immersing the deoiled PET fiber in the roughening solution at 35 ℃ for 4min, taking out the PET fiber, putting the PET fiber into oxalic acid solution with the concentration of 12g/L, placing the PET fiber at the water bath temperature of 30 ℃ for 3min, and then washing the PET fiber for 1 time by using deionized water;
step 3): to 500ml of deionized water, 4g of SnCl was added2Adding 18ml of HCl with the concentration of 38% into the solid particles, stirring and dissolving to form uniform sensitizing solution, immersing the PET fibers treated in the step 2) into the sensitizing solution, and placing the PET fibers at the water bath temperature of 35 ℃ for 4 min;
step 4): to 200ml of deionized water, 0.08g of PdCl was added2Stirring and dissolving solid powder and 3ml of HCl with the concentration of 38 percent to form uniform activation solution, and preparing the PET fiber treated by the step 3)Immersing vitamin in activating solution, and placing at 35 deg.C water bath temperature for 4 min;
step 5): dissolve 8g of CuSO in 140ml of deionized water4Dissolving 0.9g of NiSO in 40ml of deionized water4·6H2Dissolving 42g of sodium tartrate in 140ml of deionized water, dissolving 6.5g of NaOH in 40ml of deionized water, sequentially pouring the CuSO4 solution, the NiSO4 solution, the sodium tartrate solution and the NaOH solution into a 500ml volumetric flask, adding 7ml of HCHO, and finally adding deionized water to 500ml to obtain a chemical copper plating solution, putting the PET fibers treated in the step 4) into the copper plating solution, and placing the PET fibers at the water bath temperature of 33 ℃ for 25 min;
step 6): weighing 5.5g of nano titanium dioxide powder, dispersing the nano titanium dioxide powder in 145ml of NaOH solution, fully stirring the mixture, pouring the mixture into a reaction kettle, placing the reaction kettle in a drying oven at 130 ℃ for reacting for 36 hours, placing the reaction kettle in a centrifuge at the rotating speed of 3000r/s for centrifuging to obtain white precipitate, washing the white precipitate by using a solution with the concentration of 0.1mol/LHCl until the PH is 1.5, stirring the mixture for 24 hours at normal temperature, ultrasonically treating the mixture for 1.5 hours, placing the mixture in the centrifuge at the rotating speed of 3000r/s for obtaining the white precipitate again, washing the white precipitate to be neutral by using deionized water, and placing the mixture in the drying oven at 70 ℃ for drying to obtain a titanium dioxide;
step 7): preparation H2TCPP-TNT binary complex: weighing 15mg protoporphyrin, dissolving the protoporphyrin in 100ml N 'N-dimethylformamide, adding 0.8g titanium dioxide nanotube obtained in the step 6), fully stirring to obtain a mixed solution, pouring the mixed solution into a 250ml single-neck flask, heating to 120 ℃ in a dark environment, reacting for 5 hours, carrying out vacuum filtration to obtain a precipitate, washing with 15ml N' N-dimethylformamide, washing with deionized water for 2 minutes, and finally drying in a 60 ℃ oven to obtain H2TCPP-TNT powder;
step 8): laying a layer of H with the thickness of 1mm on clean and smooth white paper2TCPP-TNT powder, horizontally placing the PET fiber obtained in the step 5) on the powder, scattering a layer of H2TCPP-TNT powder on the PET fiber, coating silicon rubber on the PET fiber, placing the PET fiber in a 100 ℃ oven to be dried for 30min, curing the silicon rubber to obtain the composite fiber capable of generating current under the irradiation of sunlight, wherein the silicon rubber comprises a main agent and a curing agent,the mass ratio of the main agent to the curing agent is 3: 1.
Example 2
The invention relates to a preparation method of a fiber for generating photocurrent by sunlight, which comprises the following preparation steps:
step 1): adding PET fiber with smooth surface into sodium hydroxide solution with concentration of 0.12mol/L, and placing at water bath temperature of 65 ℃ for 4 min;
step 2): to 500ml of deionized water, 7.5g of KMnO4 solid particles were added, dissolved with stirring, and 20ml of 98% H was added2SO4Magnetically stirring for 12min to form uniform roughening solution, immersing the deoiled PET fiber in the roughening solution at 40 ℃ for 5min, taking out the PET fiber, putting the PET fiber into oxalic acid solution with the concentration of 12g/L, placing the PET fiber at the water bath temperature of 35 ℃ for 4min, and then washing the PET fiber for 1 time by using deionized water;
step 3): 5g of SnCl was added to 500ml of deionized water2Adding 20ml of HCl with the concentration of 38% into the solid particles, stirring and dissolving to form uniform sensitizing solution, immersing the PET fibers treated in the step 2) into the sensitizing solution, and placing the PET fibers at the water bath temperature of 40 ℃ for 4.5 min;
step 4): to 200ml of deionized water, 0.09g of PdCl was added2Stirring and dissolving solid powder and 3.5ml of HCl with the concentration of 38% to form uniform activation liquid, immersing the PET fibers treated in the step 3) in the activation liquid, and placing the PET fibers at the water bath temperature of 40 ℃ for 5 min;
step 5): dissolve 10g of CuSO in 150ml of deionized water4Dissolving 1.0g of NiSO in 45ml of deionized water4·6H2O, dissolving 45g of sodium tartrate in 150ml of deionized water, dissolving 8g of NaOH in 45ml of deionized water, and adding the above CuSO4Solution, NiSO4Sequentially pouring the solution, the sodium tartrate solution and the NaOH solution into a 500ml volumetric flask, then adding 7.5ml of HCHO, and finally adding deionized water to 500ml to obtain a chemical copper plating solution, putting the PET fibers treated in the step 4) into the copper plating solution, and placing the PET fibers at the water bath temperature of 35 ℃ for 30 min;
step 6): weighing 6g of nano titanium dioxide powder, dispersing the nano titanium dioxide powder in 150ml of NaOH solution, fully stirring the solution, pouring the solution into a reaction kettle, placing the reaction kettle in a 135 ℃ drying oven for reacting for 36 hours, placing the reaction kettle in a 3000r/s centrifugal machine for centrifuging to obtain a white precipitate, washing the white precipitate by using a 0.15mol/LHCl solution until the pH value is 1.5, stirring the solution for 24.5 hours at normal temperature, ultrasonically treating the solution for 1.5 hours, placing the solution in a 3000r/s centrifugal machine for obtaining the white precipitate again, washing the white precipitate to be neutral by using deionized water, and placing the precipitate in a 75 ℃ drying oven for drying to obtain a titanium dioxide nanotube;
step 7): preparation H2TCPP-TNT binary complex: weighing 17mg protoporphyrin, dissolving in 100ml N 'N-dimethylformamide, adding 0.9g titanium dioxide nanotube obtained in the step 6), fully stirring to obtain a mixed solution, pouring the mixed solution into a 250ml single-neck flask, heating to 120 ℃ in dark environment, reacting for 5.5H, vacuum-filtering to obtain a precipitate, washing with 20ml N' N-dimethylformamide, washing with deionized water for 2.5min, and finally drying in a 65 ℃ oven to obtain H2TCPP-TNT powder;
step 8): laying a layer of H with the thickness of 1.5mm on clean and smooth white paper2TCPP-TNT powder, laying the PET fiber obtained in the step 5) on the powder, and then scattering a layer of H on the PET fiber2Coating silicon rubber on PET fiber, placing in a drying oven at 105 ℃ for drying for 35min, and curing the silicon rubber to obtain the composite fiber capable of generating current under the irradiation of sunlight, wherein the silicon rubber comprises a main agent and a curing agent, and the mass ratio of the main agent to the curing agent is 3: 1.
Example 3
The invention relates to a preparation method of a fiber for generating photocurrent by sunlight, which comprises the following preparation steps:
step 1): adding PET fiber with smooth surface into sodium hydroxide solution with concentration of 0.15mol/L, and placing at 70 deg.C water bath temperature for 5 min;
step 2): to 500ml of deionized water, 8g of KMnO4 solid particles were added, dissolved with stirring, and 22ml of 98% H was added2SO4Magnetically stirring for 15min to form uniform roughening solution, immersing deoiled PET fiber in 45 deg.C roughening solution for 6min, taking out PET fiber, and adding grass with concentration of 12g/LPlacing in acid solution, placing at 40 deg.C water bath temperature for 5min, and cleaning with deionized water for 2 times;
step 3): to 500ml of deionized water, 6g of SnCl was added2Adding 22ml of HCl with the concentration of 38% into the solid particles, stirring and dissolving to form uniform sensitizing solution, immersing the PET fibers treated in the step 2) in the sensitizing solution, and placing the PET fibers at the water bath temperature of 45 ℃ for 6 min;
step 4): in 200ml of deionized water, 0.1g of PdCl was added2Stirring and dissolving solid powder and 4ml of HCl with the concentration of 38% to form uniform activation liquid, immersing the PET fibers treated in the step 3) in the activation liquid, and placing the PET fibers at the water bath temperature of 45 ℃ for 6 min;
step 5): dissolve 12g of CuSO in 160ml of deionized water4Dissolving 1.1g of NiSO in 50ml of deionized water4·6H2O, dissolving 48g of sodium tartrate in 160ml of deionized water, dissolving 7.5g of NaOH in 50ml of deionized water, sequentially pouring the CuSO4 solution, the NiSO4 solution, the sodium tartrate solution and the NaOH solution into a 500ml volumetric flask, adding 8ml of HCHO, and finally adding deionized water to 500ml to obtain a chemical copper plating solution, putting the PET fibers treated in the step 4) into the copper plating solution, and placing the PET fibers at the water bath temperature of 37 ℃ for 35 min;
step 6): weighing 6.5g of nano titanium dioxide powder, dispersing in 155ml of NaOH solution, fully stirring, pouring into a reaction kettle, placing the reaction kettle in an oven at 140 ℃ for reacting for 36h, placing the reaction kettle in a centrifuge at the rotating speed of 3000r/s for centrifuging to obtain a white precipitate, washing the white precipitate with a 0.2mol/LHCl solution until the PH is 1.5, stirring for 25h at normal temperature, ultrasonically treating for 1.5h, placing the reaction kettle in the centrifuge at the rotating speed of 3000r/s for obtaining the white precipitate again, washing the white precipitate to be neutral with deionized water, and placing the reaction kettle in the oven at 80 ℃ for drying to obtain a titanium dioxide nanotube;
step 7): preparation H2TCPP-TNT binary complex: weighing 20mg protoporphyrin, dissolving in 100ml N' N-dimethylformamide, adding 1.0g titanium dioxide nanotube obtained in the step 6), stirring thoroughly to obtain a mixed solution, pouring the mixed solution into a 250ml single-neck flask, heating to 120 ℃ in dark environment, reacting for 5-6h, and vacuum filtering to obtain the final productWashing the precipitate with 25ml N' N-dimethylformamide, washing with deionized water for 3min, and oven drying at 70 deg.C to obtain H2TCPP-TNT powder;
step 8): laying a layer of H with the thickness of 2mm on clean and smooth white paper2Placing the PET fiber obtained in the step 5) on the TCPP-TNT powder, scattering a layer of H2TCPP-TNT powder on the PET fiber, coating silicon rubber on the PET fiber, placing the PET fiber in a drying oven at 110 ℃ for drying for 40min, and curing the silicon rubber to obtain the composite fiber capable of generating current under the irradiation of sunlight, wherein the silicon rubber comprises a main agent and a curing agent, and the mass ratio of the main agent to the curing agent is 3.5: 1.
Finally, it should be noted that the present invention is not limited to the above embodiments, and many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.

Claims (2)

1. A preparation method of a fiber for generating photocurrent by sunlight is characterized by comprising the following preparation steps:
step 1): adding PET fiber with smooth surface into sodium hydroxide solution with concentration of 0.1-0.15mol/L, and placing at water bath temperature of 60-70 deg.C for 3-5 min;
step 2): adding 7-8g KMnO into 500ml deionized water4Dissolving the solid particles with stirring, and adding 18-22ml of 98% H2SO4Magnetically stirring for 10-15min to form uniform roughening solution, immersing the deoiled PET fiber in the roughening solution at 35-45 ℃ for 4-6min, taking out the PET fiber, putting the PET fiber into oxalic acid solution with the concentration of 12g/L, placing the solution at the water bath temperature of 30-40 ℃ for 3-5min, and then washing the solution for 1-2 times by using deionized water;
step 3): adding 4-6g SnCl into 500ml deionized water2Adding 18-22ml of HCl with the concentration of 38% into the solid particles, stirring and dissolving to form uniform sensitizing solution, immersing the PET fibers treated in the step 2) into the sensitizing solution, and placing the PET fibers at the water bath temperature of 35-45 ℃ for 4-6 min;
step 4): adding 0.08-0.1g of PdCl into 200ml of deionized water2Stirring and dissolving solid powder and 3-4ml of 38% HCl to form uniform activation liquid, immersing the PET fiber treated in the step 3) in the activation liquid, and placing the PET fiber at the water bath temperature of 35-45 ℃ for 4-6 min;
step 5): dissolving 8-12g of CuSO in 160ml of 140-160ml of deionized water4Dissolving 0.9-1.1g of NiSO in 40-50ml of deionized water4·6H2O, dissolving 42-48g of sodium tartrate in 140-160ml of deionized water, dissolving 6.5-7.5g of NaOH in 40-50ml of deionized water, and mixing the CuSO4Solution, NiSO4Sequentially pouring the solution, the sodium tartrate solution and the NaOH solution into a 500ml volumetric flask, then adding 7-8ml of HCHO, and finally adding deionized water to 500ml to obtain a chemical copper plating solution, putting the PET fibers treated in the step 4) into the copper plating solution, and placing the PET fibers at the water bath temperature of 33-37 ℃ for 25-35 min;
step 6): weighing 5.5-6.5g of nano titanium dioxide powder, dispersing the nano titanium dioxide powder in 155ml of NaOH solution, fully stirring the solution, pouring the solution into a reaction kettle, placing the reaction kettle in an oven with the temperature of 130-140 ℃ for reaction for 36h, placing the reaction kettle in a centrifuge with the rotating speed of 3000r/s for centrifugation to obtain white precipitate, washing the white precipitate by using a solution with the concentration of 0.1-0.2mol/LHCl until the pH value is 1.5, stirring the solution at normal temperature for 24-25h, performing ultrasonic treatment for 1.5h, placing the solution in the centrifuge with the rotating speed of 3000r/s to obtain the white precipitate again, washing the white precipitate to be neutral by using deionized water, and placing the solution in the oven with the temperature of 70-80 ℃ for drying to obtain the titanium dioxide;
step 7): preparation H2TCPP-TNT binary complex: weighing 15-20mg protoporphyrin, dissolving in 100ml N 'N-dimethylformamide, adding 0.8-1.0g titanium dioxide nanotube obtained in the step 6), stirring fully to obtain a mixed solution, pouring the mixed solution into a 250ml single-neck flask, heating to 120 ℃ in dark environment, reacting for 5-6H, vacuum filtering to obtain a precipitate, washing with 15-25ml N' N-dimethylformamide, washing with deionized water for 2-3min, and finally drying in a 60-70 ℃ oven to obtain H2TCPP-TNT powder;
step 8): laying a layer of H with the thickness of 1-2mm on clean and smooth white paper2TCPP-TNT powder, PET fiber obtained in step 5)Laying the fiber on the powder, and then scattering a layer of H on the PET fiber2Coating silicon rubber on PET (polyethylene terephthalate) fiber, and placing the PET fiber in an oven at the temperature of 100-110 ℃ for baking for 30-40min to cure the silicon rubber to obtain the composite fiber capable of generating current under the irradiation of sunlight, wherein the silicon rubber comprises a main agent and a curing agent, and the mass ratio of the main agent to the curing agent is 3-3.5: 1.
2. A preparation method of a fiber for generating photocurrent by sunlight is characterized by comprising the following preparation steps:
step 1): adding PET fiber with smooth surface into sodium hydroxide solution with concentration of 0.12mol/L, and placing at water bath temperature of 65 ℃ for 4 min;
step 2): to 500ml of deionized water, 7.5g of KMnO was added4The solid particles were dissolved with stirring and 20ml of 98% H were added2SO4Magnetically stirring for 12min to form uniform roughening solution, immersing the deoiled PET fiber in the roughening solution at 40 ℃ for 5min, taking out the PET fiber, putting the PET fiber into oxalic acid solution with the concentration of 12g/L, placing the PET fiber at the water bath temperature of 35 ℃ for 4min, and then washing the PET fiber for 1 time by using deionized water;
step 3): 5g of SnCl was added to 500ml of deionized water2Adding 20ml of HCl with the concentration of 38% into the solid particles, stirring and dissolving to form uniform sensitizing solution, immersing the PET fibers treated in the step 2) into the sensitizing solution, and placing the PET fibers at the water bath temperature of 40 ℃ for 4.5 min;
step 4): to 200ml of deionized water, 0.09g of PdCl was added2Stirring and dissolving solid powder and 3.5ml of 38% HCl to form uniform activation liquid, immersing the PET fibers treated in the step 3) in the activation liquid, and placing the PET fibers at the water bath temperature of 40 ℃ for 5 min;
step 5): dissolve 10g of CuSO in 150ml of deionized water4Dissolving 1.0g of NiSO in 45ml of deionized water4·6H2O, dissolving 45g of sodium tartrate in 150ml of deionized water, dissolving 8g of NaOH in 45ml of deionized water, and adding the above CuSO4Solution, NiSO4The solution, the sodium tartrate solution and the NaOH solution are poured into a 500ml volumetric flask in turn, and 7.5ml HCH is addedO, finally adding deionized water to 500ml to obtain a chemical copper plating solution, putting the PET fiber treated in the step 4) into the copper plating solution, and placing the PET fiber at the water bath temperature of 35 ℃ for 30 min;
step 6): weighing 6g of nano titanium dioxide powder, dispersing in 150ml of NaOH solution, fully stirring, pouring into a reaction kettle, placing the reaction kettle in a 135 ℃ oven for reaction for 36h, placing the reaction kettle in a 3000r/s centrifuge for centrifugation to obtain a white precipitate, washing the white precipitate with 0.15mol/LHCl solution until the pH value is 1.5, stirring for 24.5h at normal temperature, performing ultrasonic treatment for 1.5h, placing the white precipitate in a 3000r/s centrifuge for secondary obtaining of the white precipitate, washing the white precipitate with deionized water to be neutral, and placing the white precipitate in a 75 ℃ oven for drying to obtain a titanium dioxide nanotube;
step 7): preparation H2TCPP-TNT binary complex: weighing 17mg protoporphyrin, dissolving in 100ml N 'N-dimethylformamide, adding 0.9g titanium dioxide nanotube obtained in the step 6), fully stirring to obtain a mixed solution, pouring the mixed solution into a 250ml single-neck flask, heating to 120 ℃ in dark environment, reacting for 5.5H, vacuum-filtering to obtain a precipitate, washing with 20ml N' N-dimethylformamide, washing with deionized water for 2.5min, and finally drying in a 65 ℃ oven to obtain H2TCPP-TNT powder;
step 8): laying a layer of H with the thickness of 1.5mm on clean and smooth white paper2TCPP-TNT powder, laying the PET fiber obtained in the step 5) on the powder, and then scattering a layer of H on the PET fiber2Coating silicon rubber on PET (polyethylene terephthalate) fibers, and placing the PET fibers in an oven at 105 ℃ for baking for 35min to cure the silicon rubber to obtain the composite fiber capable of generating current under the irradiation of sunlight, wherein the silicon rubber comprises a main agent and a curing agent, and the mass ratio of the main agent to the curing agent is 3: 1.
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