CN105970601A - Method for preparing titanium dioxide nanorod/polypyrrole/dacron compound fabric - Google Patents

Method for preparing titanium dioxide nanorod/polypyrrole/dacron compound fabric Download PDF

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CN105970601A
CN105970601A CN201610398715.6A CN201610398715A CN105970601A CN 105970601 A CN105970601 A CN 105970601A CN 201610398715 A CN201610398715 A CN 201610398715A CN 105970601 A CN105970601 A CN 105970601A
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polypyrrole
titanium dioxide
dacron
titanium
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CN105970601B (en
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徐阳
吴进明
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Zhejiang University ZJU
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/32Treating 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
    • D06M11/36Treating 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
    • D06M11/46Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic System; Titanates; Zirconates; Stannates; Plumbates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/0605Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
    • C08G73/0611Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring, e.g. polypyrroles
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32Polyesters
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/01Stain or soil resistance

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a method for preparing a titanium dioxide nanorod/polypyrrole/dacron compound fabric. The method comprises the steps of cleaning and drying a dacron fabric, and then placing the dacron fabric in alkali aqueous ammonia for surface roughness treatment; then soaking the dacron fabric in an oxidization bath, and adding pyrrole monomer aqueous solution dropwise so that a polypyrrole layer can be deposited on the surface of the dacron fabric; soaking the dacron fabric with polypyrrole deposited on the surface in prepared titanium dioxide sol, conducting lifting, drying and hydrochloric acid treatment so that a titanium dioxide seed crystal layer can be deposited on the surface of the dacron fabric, and conducting hydrochloric acid treatment and sulfuric acid treatment in sequence; preparing titanium dioxide nanorod growth-promoting media, and adding an excessive amount of titanium source so that titanium dioxide nanorods can be deposited and grown on the surface of the treated dacron fabric. Combination of the one-dimensional titanium dioxide nanorods and polypyrrole on a substrate of a flexible fabric is realized, and the obtained compound fabric has self-cleaning, anti-statistic, photocatalytic degradation and pollutant filtration functions and can be used as a flexible electrode and a flexible supercapacitor.

Description

A kind of titanium dioxide nano-rod / Polypyrrole / The preparation method of terylene compound fabric
Technical field
The present invention relates to the preparation method of a kind of titanium dioxide nano-rod/polypyrrole/terylene compound fabric, belong to energy and environment field of material technology.
Background technology
Titanium dioxide (TiO2), compared to ZnO, Fe2O3, the semiconductor light-catalyst such as ZnS, CdS there is higher chemical stability, and biocompatibility is excellent, nontoxic, the performance shown at aspects such as photocatalytic water, photochemical catalytic oxidation, photo catalytic reduction, photocatalysis synthesis of organic substance, photocatalytic degradation Organic substance, sterilizing, solaode, automatically cleaning, gas sensor and humidity sensors is noticeable, has important application prospect.But TiO2It is only capable of absorbing ultraviolet light, low to solar energy utilization ratio.Zero dimension TiO2Although nano-particle has higher photocatalytic activity, but reclaims difficult, easily cause secondary pollution of water.Therefore, preparation has the one-dimensional TiO of highlight catalytic active2Nano structure membrane is particularly important.
Conducting polymer such as polypyrrole, polyaniline, polythiophene etc. have the strongest absorption in visible region, can be as a kind of stronger electron-donating material and good hole mobile material.Therefore, conducting polymer and TiO2It is combined and can improve sunlight utilization rate.Additionally, TiO2It is combined with conducting polymer that to prepare ultracapacitor be also current study hotspot.Polypyrrole has preferable electric conductivity, relatively low oxidizing potential, is more easily-synthesized compared to other conducting polymers, and environmental stability is good, have a extensive future at aspects such as electrode material, electrochemistry, biosensor, anti-static material and electroluminescent materials, receive significant attention.
At present, multiple TiO is had been carried out2One-dimensional nano structure is compound, such as patent CN with conductive rigid substrate, metallic substrates and electro-conductive glass substrate 102881455A discloses composite Ti O on FTO electro-conductive glass and ITO electro-conductive glass2The method of nanotube;Patent CN 102418148A discloses depositing Ti O in the rigid conductive substrates such as electro-conductive glass, titanium sheet and stainless steel substrates2The method of nano-tube film further electro-deposition polypyrrole, for opto-electronic conversion field.But, the one-dimensional TiO in addition to nanotube2Nanostructured and flexible substrates particularly the compound of conductive flexible substrate have no report.
Textile fabric has extraordinary pliability, can be compiled into variously-shaped, be suitable as flexible substrate.But general textile fabric is non-conductive, the flexible fabric that the easiest preparation has good electrical chemical property becomes subject matter.Although ITO has been coated in polyethylene terephthalate (ITO/PET) or ITO is coated in PEN (ITO/PEN) prepare conductive fabric obtain conductive flexible substrate technology, but relatively costly.
Summary of the invention
Because the deficiency of prior art, it is an object of the invention to provide a kind of TiO2The preparation method of nanometer rods/polypyrrole/terylene compound fabric.
The preparation method of the titanium dioxide nano-rod/polypyrrole/terylene compound fabric of the present invention, comprises the following steps:
(1) ethylenediamine, sodium hydroxide and accelerator 1631 are dissolved configuration alkali amine aqueous solution in deionized water, and making the mass concentration of ethylenediamine in alkali amine aqueous solution is 2%, and the mass concentration of sodium hydroxide is 28%, and the mass concentration of accelerator 1631 is 0.08%;Dacron is cleaned with acetone, second alcohol and water respectively, dries, then dacron is immersed in alkali amine aqueous solution by 1:30 ~ 1:50 bath raio, at 55 ~ 75 DEG C, react 10 ~ 20 Min, washing, it is dried, obtains the dacron that rough surfaceization processes;
(2) by FeCl3Or Fe2(SO4)3With 1,5-naphthalenedisulfonic acid is dissolved in deionized water, configures oxidation bath, makes FeCl in oxidation bath3Or Fe2(SO4)3Concentration be respectively 0.09 M or 0.045 M, the concentration of 1,5-naphthalenedisulfonic acid is 0.012M, is immersed in oxidation bath by the dacron processed through rough surfaceization;
Configuration concentration is 0.01 ~ 0.15 M pyrrole monomer aqueous solution, under agitation, pyrrole monomer aqueous solution is dropwise added drop-wise in oxidation bath, the volume ratio of oxidation bath and pyrrole monomer aqueous solution is 0.125 ~ 1, drip after complete follow-up continuous stirring fully reacts, take out, clean, and be dried at 25 ~ 40 DEG C, obtain polypyrrole/terylene compound fabric;
(3) at 0 ~ 10 DEG C, by butyl titanate, water, nitric acid and ethanol 1:1:0.1:9.25 in molar ratio
It is sufficiently mixed, obtains TiO 2 sol, polypyrrole/terylene compound fabric that step (2) prepares is immersed in TiO 2 sol 6 ~ 36 H, then with 100 ~ 400 mm/min speed liftings, under the conditions of 60 ~ 80 DEG C, it is dried at least 12h;
(4) polypyrrole processed through step (3)/terylene compound fabric is put in the hydrochloric acid solution that concentration is 0.1 ~ 0.2 M, at 60 ~ 80 DEG C, react 24 ~ 36h, washing, it is dried, then puts in the sulfuric acid solution that pH value is 1.5 ~ 3.5, at 60 ~ 80 DEG C, react 24 ~ 48 h, washing, is dried;
(5) to mass concentration be 20 ~ 30 Adding hydrochloric acid and tripolycyanamide in the hydrogen peroxide solution of %, making the concentration of hydrochloric acid in solution is 0.48M, and the mass concentration of tripolycyanamide is 0.06% ~ 0.1%, adds the titanium sponge of excess or titanium valve or titanium sheet as titanium source, 60 ~ 80 React 12 h at DEG C, take the growth-promoting media that upper liquid is titanium dioxide nano-rod;Will be in polypyrrole/terylene compound fabric that step (4) process immerse the growth-promoting media of titanium dioxide nano-rod, the titanium sponge of addition excess or titanium valve or titanium sheet are as supplementary titanium source, 60 ~ 80 React 12 ~ 48 h at DEG C, take out washing, be dried, obtain titanium dioxide nano-rod/polypyrrole/terylene compound fabric.
Advantages of the present invention:
Preparation method simplicity of the present invention is controlled, and cost is relatively low.The present invention is uniform deposition polypyrrole on nonconducting dacron, and making polypyrrole with to have good flexible dacron compound becomes conductive substrates, deposition growing TiO on this polypyrrole/dacron further2One-dimensional nano structure.Present invention achieves one-dimensional titanium dioxide nanorod structure and polypyrrole being combined on flexible fabric substrate, the compound fabric obtained has the functions such as automatically cleaning, antistatic, photocatalytic degradation and filtering contaminants, and can be used as flexible electrode and flexible super capacitor.
Accompanying drawing explanation
Fig. 1 is the field emission scanning electron microscope photo on the titanium dioxide nano-rod/polypyrrole/terylene compound fabric surface of embodiment 1 preparation.
Fig. 2 is the field emission scanning electron microscope photo on the titanium dioxide nano-rod/polypyrrole/terylene compound fabric surface of embodiment 2 preparation.
Fig. 3 is the XRD figure spectrum on the titanium dioxide nano-rod/polypyrrole/terylene compound fabric surface of embodiment 3 preparation.
Fig. 4 is the field emission scanning electron microscope photo on the titanium dioxide nano-rod/polypyrrole/terylene compound fabric surface of embodiment 4 preparation.
Detailed description of the invention
The present invention is expanded on further below in conjunction with embodiment, but the present invention is not limited solely to following embodiment.
Embodiment 1
(1) ethylenediamine, sodium hydroxide and accelerator 1631 are dissolved configuration alkali amine aqueous solution in deionized water, and making the mass concentration of ethylenediamine in alkali amine aqueous solution is 2%, and the mass concentration of sodium hydroxide is 28%, and the mass concentration of accelerator 1631 is 0.08%;Choosing the dacron that specification is 75 D × 120 D is sample, takes size 5 × 5 cm2Sample wash 1 time through acetone respectively, ethanol is washed 3 times and deionization and is washed 3 times, dries, then
Dacron is immersed in alkali amine aqueous solution by 1:30 bath raio, at 75 DEG C, reacts 10 min, washing, it is dried.
(2) by FeCl3With 1,5-naphthalenedisulfonic acid is dissolved in deionized water, configures oxidation bath 30 mL, makes FeCl in oxidation bath3Concentration be 0.09 M, the concentration of 1,5-naphthalenedisulfonic acid is 0.012 M.Dacron through above-mentioned process is immersed in 30 min in oxidation bath;
Configuration concentration is 0.05 M pyrrole monomer aqueous solution 60 mL, under agitation, is dropwise added drop-wise in oxidation bath by pyrrole monomer aqueous solution, drips complete follow-up continuous stirring reaction 2 h, takes out, washing, and 25 DEG C are dried.
(3) at 4 DEG C, it is that 1:1:0.1:9.25 is sufficiently mixed configuration colloidal sol by the mol ratio of butyl titanate, water, nitric acid and ethanol, sample after step (2) processes is immersed in 24 h in this colloidal sol, then with 100 mm/min speed liftings, at 80 DEG C, is dried 24 h.
(4) sample processed through step (3) being immersed in concentration is in 0.15 M hydrochloric acid solution, reacts 24 h at 60 DEG C, washing, is dried, then puts in pH=2.5 sulfuric acid solution, react 48 h at 80 DEG C, and washing is dried.
(5) adding hydrochloric acid and tripolycyanamide in the hydrogen peroxide solution that mass concentration is 30 %, making the concentration of hydrochloric acid in solution is 0.48 M, and the mass concentration of tripolycyanamide is 0.06 %, the titanium sheet of addition excess, as titanium source, reacts 12 h at 80 DEG C.Taking upper liquid is titanium dioxide nano-rod growth-promoting media, the sample processed through step (4) is immersed in this titanium dioxide nano-rod growth-promoting media, add the titanium sponge of excess as supplementary titanium source, 24 h are reacted at 80 DEG C, washing, it is dried, obtains titanium dioxide nano-rod/polypyrrole/terylene compound fabric finished product, see Fig. 1.
Embodiment 2
(1) ethylenediamine, sodium hydroxide and accelerator 1631 are dissolved configuration alkali amine aqueous solution in deionized water, and making the mass concentration of ethylenediamine in alkali amine aqueous solution is 2%, and the mass concentration of sodium hydroxide is 28%, and the mass concentration of accelerator 1631 is 0.08%;Choosing the dacron that specification is 75 D × 120 D is sample, takes size 5 × 5 cm2Sample wash 1 time through acetone respectively, ethanol is washed 3 times and deionization and is washed 3 times, dries, then
Dacron is immersed in alkali amine aqueous solution by 1:50 bath raio, at 55 DEG C, reacts 20 min, washing, it is dried.
(2) by Fe2(SO4)3With 1,5-naphthalenedisulfonic acid is dissolved in deionized water, configures oxidation bath 15 mL, makes Fe in oxidation bath2(SO4)3Concentration be 0.045 M, the concentration of 1,5-naphthalenedisulfonic acid is 0.012 M.Dacron through above-mentioned process is immersed in oxidation bath 10 min;
Configuration concentration is 0.10 M pyrrole monomer aqueous solution 50 mL, under agitation, is dropwise added drop-wise in oxidation bath by pyrrole monomer aqueous solution, drips complete follow-up continuous stirring reaction 4 h, takes out, washing, and 40 DEG C are dried.
(3) at 0 DEG C, it is that 1:1:0.1:9.25 is sufficiently mixed configuration colloidal sol by the mol ratio of butyl titanate, water, nitric acid and ethanol, sample after step (2) processes is immersed in 24 h in this colloidal sol, then with 300 mm/min speed liftings, at 80 DEG C, is dried 24 h.
(4) sample processed through step (3) being immersed in concentration is in 0.10 M hydrochloric acid solution, reacts 24 h at 70 DEG C, washing, is dried, then puts in pH=2.5 sulfuric acid solution, react 48 h at 80 DEG C, and washing is dried.
(5) adding hydrochloric acid and tripolycyanamide in the hydrogen peroxide solution that mass concentration is 30 %, making the concentration of hydrochloric acid in solution is 0.48 M, and the mass concentration of tripolycyanamide is 0.1 %, and the titanium sheet of addition excess, as titanium source, reacts 12 h at 80 DEG C.Taking upper liquid is titanium dioxide nano-rod growth-promoting media, the sample processed through step (4) is immersed in this titanium dioxide nano-rod growth-promoting media, add the titanium sponge of excess as supplementary titanium source, 48h is reacted at 80 DEG C, washing, it is dried, obtains titanium dioxide nano-rod/polypyrrole/terylene compound fabric finished product, see Fig. 2.
Embodiment 3
(1) ethylenediamine, sodium hydroxide and accelerator 1631 are dissolved configuration alkali amine aqueous solution in deionized water, and making the mass concentration of ethylenediamine in alkali amine aqueous solution is 2%, and the mass concentration of sodium hydroxide is 28%, and the mass concentration of accelerator 1631 is 0.08%;Choosing the dacron that specification is 75 D × 75 D is sample, takes size 5 × 5 cm2Sample wash 1 time through acetone respectively, ethanol is washed 3 times and deionization and is washed 3 times, dries, then
Dacron is immersed in alkali amine aqueous solution by 1:30 bath raio, at 75 DEG C, reacts 10 min, washing, it is dried.
(2) by Fe2(SO4)3With 1,5-naphthalenedisulfonic acid is dissolved in deionized water, configures oxidation bath 20 mL, makes Fe in oxidation bath2(SO4)3Concentration be 0.045M, the concentration of 1,5-naphthalenedisulfonic acid is 0.012 M.Dacron through above-mentioned process is immersed in oxidation bath 20 min;
Configuration concentration is 0.15 M pyrrole monomer aqueous solution 30 mL, under agitation, is dropwise added drop-wise in oxidation bath by pyrrole monomer aqueous solution, drips complete follow-up continuous stirring reaction 6 h, takes out, washing, and 40 DEG C are dried.
(3) at 0 DEG C, it is that 1:1:0.1:9.25 is sufficiently mixed configuration colloidal sol by the mol ratio of butyl titanate, water, nitric acid and ethanol, sample after step (2) processes is immersed in 24 h in this colloidal sol, then with 300 mm/min speed liftings, at 80 DEG C, is dried 24 h.
(4) sample processed through step (3) being immersed in concentration is in 0.15 M hydrochloric acid solution, reacts 24 h at 60 DEG C, washing, is dried, then puts in pH=2 sulfuric acid solution, react 24 h at 80 DEG C, and washing is dried.
(5) adding hydrochloric acid and tripolycyanamide in the hydrogen peroxide solution that mass concentration is 20 %, making the concentration of hydrochloric acid in solution is 0.48 M, and the mass concentration of tripolycyanamide is 0.1 %, and the titanium sponge of addition excess, as titanium source, reacts 12 h at 80 DEG C.Taking upper liquid is titanium dioxide nano-rod growth-promoting media, the sample processed through step (4) is immersed in this titanium dioxide nano-rod growth-promoting media, add the titanium sponge of excess as supplementary titanium source, 48h is reacted at 60 DEG C, washing, it is dried, obtains titanium dioxide nano-rod/polypyrrole/terylene compound fabric finished product.The XRD result of Fig. 3 shows, gained titanium dioxide crystal is good, and its phase composition is anatase, rutile and brockite.
Embodiment 4
(1) ethylenediamine, sodium hydroxide and accelerator 1631 are dissolved configuration alkali amine aqueous solution in deionized water, and making the mass concentration of ethylenediamine in alkali amine aqueous solution is 2%, and the mass concentration of sodium hydroxide is 28%, and the mass concentration of accelerator 1631 is 0.08%;Choosing the dacron that specification is 75 D × 75 D is sample, takes size 5 × 5 cm2Sample wash 1 time through acetone respectively, ethanol is washed 3 times and deionization and is washed 3 times, dries, then
Dacron is immersed in alkali amine aqueous solution by 1:30 bath raio, at 75 DEG C, reacts 10 min, washing, it is dried.
(2) by FeCl3With 1,5-naphthalenedisulfonic acid is dissolved in deionized water, configures oxidation bath 20 mL, makes FeCl in oxidation bath3Concentration be 0.09M, the concentration of 1,5-naphthalenedisulfonic acid is 0.012 M.Dacron through above-mentioned process is immersed in 30 min in oxidation bath;
Configuration concentration is 0.15 M pyrrole monomer aqueous solution 20 mL, under agitation, is dropwise added drop-wise in oxidation bath by pyrrole monomer aqueous solution, drips complete follow-up continuous stirring reaction 1 h, takes out, washing, and 30 DEG C are dried.
(3) at 4 DEG C, it is that 1:1:0.1:9.25 is sufficiently mixed configuration colloidal sol by the mol ratio of butyl titanate, water, nitric acid and ethanol, sample after step (2) processes is immersed in 24 h in this colloidal sol, then with 100 mm/min speed liftings, at 80 DEG C, is dried 24 h.
(4) sample processed through step (3) being immersed in concentration is in 0.15 M hydrochloric acid solution, reacts 24 h at 60 DEG C, washing, is dried, then puts in pH=1.5 sulfuric acid solution, react 38 h at 60 DEG C, and washing is dried.
(5) adding hydrochloric acid and tripolycyanamide in the hydrogen peroxide solution that mass concentration is 20 %, making the concentration of hydrochloric acid in solution is 0.48 M, and the mass concentration of tripolycyanamide is 0.08 %, the titanium valve of addition excess, as titanium source, reacts 12 h at 80 DEG C.Taking upper liquid is titanium dioxide nano-rod growth-promoting media, the sample processed through step (4) is immersed in this titanium dioxide nano-rod growth-promoting media, add the titanium sponge of excess as supplementary titanium source, 36 h are reacted at 70 DEG C, washing, it is dried, obtains titanium dioxide nano-rod/polypyrrole/terylene compound fabric finished product, see Fig. 4.

Claims (1)

1. a preparation method for titanium dioxide nano-rod/polypyrrole/terylene compound fabric, comprises the following steps:
(1) ethylenediamine, sodium hydroxide and accelerator 1631 are dissolved configuration alkali amine aqueous solution in deionized water, and making the mass concentration of ethylenediamine in alkali amine aqueous solution is 2%, and the mass concentration of sodium hydroxide is 28%, and the mass concentration of accelerator 1631 is 0.08%;Dacron is cleaned with acetone, second alcohol and water respectively, dries, then dacron is immersed in alkali amine aqueous solution by 1:30 ~ 1:50 bath raio, at 55 ~ 75 DEG C, react 10 ~ 20 min, washing, be dried, obtain the dacron that rough surfaceization processes;
(2) by FeCl3Or Fe2(SO4)3With 1,5-naphthalenedisulfonic acid is dissolved in deionized water, configures oxidation bath, makes FeCl in oxidation bath3Or Fe2(SO4)3Concentration be respectively 0.09 M or 0.045 M, the concentration of 1,5-naphthalenedisulfonic acid is 0.012M, is immersed in oxidation bath by the dacron processed through rough surfaceization;
Configuration concentration is 0.01 ~ 0.15 M pyrrole monomer aqueous solution, under agitation, pyrrole monomer aqueous solution is dropwise added drop-wise in oxidation bath, the volume ratio of oxidation bath and pyrrole monomer aqueous solution is 0.125 ~ 1, drip after complete follow-up continuous stirring fully reacts, take out, clean, and be dried at 25 ~ 40 DEG C, obtain polypyrrole/terylene compound fabric;
(3) at 0 ~ 10 DEG C, by butyl titanate, water, nitric acid and ethanol 1:1:0.1:9.25 in molar ratio
It is sufficiently mixed, obtains TiO 2 sol, polypyrrole/terylene compound fabric that step (2) prepares is immersed in 6 ~ 36 h in TiO 2 sol, then with 100 ~ 400 Mm/min speed lifts, and is dried at least 12h under the conditions of 60 ~ 80 DEG C;
(4) polypyrrole processed through step (3)/terylene compound fabric is put in the hydrochloric acid solution that concentration is 0.1 ~ 0.2 M, at 60 ~ 80 DEG C, react 24 ~ 36h, washing, it is dried, then puts in the sulfuric acid solution that pH value is 1.5 ~ 3.5, at 60 ~ 80 DEG C, react 24 ~ 48 h, washing, is dried;
(5) in the hydrogen peroxide solution that mass concentration is 20 ~ 30 %, hydrochloric acid and tripolycyanamide are added, making the concentration of hydrochloric acid in solution is 0.48M, the mass concentration of tripolycyanamide is 0.06% ~ 0.1%, add excessive titanium sponge or titanium valve or titanium sheet as titanium source, at 60 ~ 80 DEG C, react 12 h, take the growth-promoting media that upper liquid is titanium dioxide nano-rod;Will be in polypyrrole/terylene compound fabric that step (4) process immerses the growth-promoting media of titanium dioxide nano-rod, add excessive titanium sponge or titanium valve or titanium sheet as supplementary titanium source, 12 ~ 48 h are reacted at 60 ~ 80 DEG C, take out washing, it is dried, obtains titanium dioxide nano-rod/polypyrrole/terylene compound fabric.
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CN106698583B (en) * 2017-02-23 2019-10-25 西南大学 A kind of preparation method of super-hydrophobic melamine sponge absorbent-type water-oil separating material and products thereof and application
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CN109731617A (en) * 2018-12-13 2019-05-10 东莞理工学院 A kind of Fe3O4/ polypyrrole/polyaniline/TiO2The preparation method of/ZnO composite material
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CN109622066A (en) * 2018-12-29 2019-04-16 东华大学 A kind of fabric/poly- nitrogen/polyaniline/titanium dioxide catalysis material preparation method
CN112704960A (en) * 2020-12-07 2021-04-27 盐城工学院 Preparation method of composite filter material
CN113602014A (en) * 2021-06-16 2021-11-05 苏州甘纳纺织有限公司 Printing and embossing synchronous forming method for polyester composite fabric
CN114481623A (en) * 2022-02-09 2022-05-13 孙秋宁 Anti-mosquito fabric and preparation method thereof
CN115491921A (en) * 2022-09-28 2022-12-20 航天特种材料及工艺技术研究所 Alumina fiber heat-insulating material and preparation method thereof
CN115491921B (en) * 2022-09-28 2024-01-26 航天特种材料及工艺技术研究所 Alumina fiber heat insulation material and preparation method thereof

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