CN101845746A - Method for modifying surface of polyester fabric with titanium tetrachloride - Google Patents
Method for modifying surface of polyester fabric with titanium tetrachloride Download PDFInfo
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- CN101845746A CN101845746A CN 201010192612 CN201010192612A CN101845746A CN 101845746 A CN101845746 A CN 101845746A CN 201010192612 CN201010192612 CN 201010192612 CN 201010192612 A CN201010192612 A CN 201010192612A CN 101845746 A CN101845746 A CN 101845746A
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Abstract
The invention discloses a method for modifying the surface of polyester fabric with titanium tetrachloride; the polyester fabric is ultrasonically oscillated and cleaned by deionized water and ethanol under the condition of 60 to 90DEG C; the polyester fabric and the titanium tetrachloride are weighed by the mass ratio of 2 to 4:1, and the titanium tetrachloride is dissolved in the deionized water by the volume ratio of 1:10 to 100 of the deionized water to the titanium tetrachloride; then the polyester fabric is soaked into titanium tetrachloride solution for 1 to 3min, added into a high-temperature high-pressure reactor, filled by the deionized water to 60 to 80 percent of the volume of the reactor, sealed, put into a 110 to 140DEG C oven to be treated for 3 to 6h; and the polyester fabric after reaction is washed by washing fluid for 10 to 20min under the condition of 70 to 90DEG C by the bath ratio of 1:30 to 50, repeatedly washed by hot and cold water, dried or naturally aired to obtain the modified polyester fabric. The method has the advantages of safety, no pollution, high production efficiency, convenient operation, raw material saving, and no high impact on the touch feel, the permeability and other properties of the polyester fabric.
Description
Technical field
The invention belongs to function textile material technical field, relate to a kind of method of modifying of dacron, be specifically related to a kind of method that adopts titanium tetrachloride the dacron surface to be carried out modification.
Background technology
Nano-titanium dioxide powder is as important inorganic functional material, have higher photocatalytic activity, good weather fastness and stronger ultraviolet screener ability, and can produce peculiar colour effect, enjoy people to pay close attention in fields such as wastewater treatment, sun-proof skin care, coating, sensor, function ceramics and photochemical catalysts.But still be faced with a series of problem, as the preparation process complexity, the cost height is difficult for disperseing in apolar medium, easily cohesion in polarizable medium, and these shortcomings directly affect the performance of its performance.
The existing method that modification is carried out on the dacron surface mainly contains two kinds.The one, preparation contains the functional fiber of nano particle, promptly in spinning process with nanoparticulate dispersed in the chemical fibre raw material, be spun to fibre again, its advantage is a consistency of performance, and shortcoming is that nano particle and polymeric material compatibility are relatively poor, and nanoparticulate dispersed is inhomogeneous, agglomeration is serious, most of nanoparticles embedded in fibrous matrix, the nano particle of fiber surface seldom, therefore functional declining to a great extent; The 2nd, adopt postfinishing process to put nano particle in order fabric face, usually need to use raw materials such as adhesive and auxiliary agent, therefore be faced with the problem of nanoparticle agglomerates too, and the fabric wash resistant fastness after the arrangement is bad, the serviceability of fabric is affected, the obvious variation of feel.How directly to prepare nano particle at the textile fabric matrix surface is a difficult problem of being badly in need of solution in the textile industry.
Summary of the invention
The purpose of this invention is to provide a kind of method that adopts titanium tetrachloride that modification is carried out on the dacron surface, solved the easy reunion of nano particle of existing method of modifying and the problem of coated fabric feel difference.
The technical solution adopted in the present invention is, a kind of method that adopts titanium tetrachloride that modification is carried out on the dacron surface is specifically implemented according to following steps:
Step 1: the dacron that will treat modification temperature be under 60～90 ℃ of conditions respectively with deionized water and concentration be 95% absolute ethyl alcohol repeatedly sonic oscillation clean dry for standby;
Step 2: according to mass ratio is dacron and titanium tetrachloride after 2～4:1 takes by weighing the processing that step 1 obtains, according to the volume ratio deionized water: titanium tetrachloride is 1:10～100, the titanium tetrachloride that takes by weighing is dissolved in deionized water, obtain titanium tetrachloride aqueous solution, dacron after the processing that will take by weighing is immersed in 1～3min in the titanium tetrachloride aqueous solution then, the titanium tetrachloride aqueous solution that is impregnated with dacron is added in the high-temperature high-pressure reaction kettle, and be filled to 60～80% of reactor volume with deionized water, sealing, it is that 110～140 ℃ baking oven is dried 3～6h that the reactor of good seal is put into temperature, and question response finishes the back and takes out dacron;
Step 3: will go up the reacted dacron that obtains of step, with the bath raio of 1:30～50, temperature be under 70～90 ℃ of conditions with cleaning solution washing 10～20min, use heat, cold water cyclic washing then, oven dry or dry naturally obtains the dacron after the modification.
Characteristics of the present invention also are,
The cleaning solution in the step 3 is wherein formed by the soda ash of the solid soap flakes of 2g/L, 2g/L is water-soluble.
The invention has the beneficial effects as follows, adopt hydrothermal technique to use titanium tetrachloride directly at polyester fabric fibers area load nano-titanium dioxide film, realized polyester fabric fibers surface clad nano titanium dioxide powder, can effectively prevent the reunion of nano-titanium dioxide powder, significantly increased the contact area of nano titanium oxide and process object, by control reaction temperature and time, technological parameters such as titanium tetrachloride and deionized water consumption, optimized finishing technique, this method is saved raw material, easy and simple to handle, prolonged wash resistant.Test result shows that the dacron after the titanium tetrachloride modification still has excellent uvioresistant and anti-microbial property through after 30 washings.
Description of drawings
Fig. 1 is the sem photograph before the dacron titanium tetrachloride hydrothermal modification;
Fig. 2 is the sem photograph after adopting the inventive method to dacron titanium tetrachloride hydrothermal modification;
Fig. 3 is to X-ray diffraction curve before the dacron titanium tetrachloride hydrothermal modification, after the modification;
Fig. 4 is the ultraviolet reflection curve of spectrum before the embodiment of the invention 1 dacron titanium tetrachloride hydrothermal modification, after the modification;
Fig. 5 is the ultraviolet reflection curve of spectrum before the embodiment of the invention 2 dacron titanium tetrachloride hydrothermal modifications, after the modification;
Fig. 6 is the ultraviolet reflection curve of spectrum before the embodiment of the invention 3 dacron titanium tetrachloride hydrothermal modifications, after the modification.
The specific embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
The method that the present invention adopts titanium tetrachloride that modification is carried out on the dacron surface, specifically implement according to following steps:
Step 1: the dacron that will treat modification temperature be under 60～90 ℃ of conditions respectively with deionized water and concentration be 95% absolute ethyl alcohol repeatedly sonic oscillation clean dry for standby then.
Step 2: according to mass ratio is dacron and titanium tetrachloride after 2～4:1 takes by weighing the processing that step 1 obtains, according to the volume ratio deionized water: titanium tetrachloride is 1:10～100, the titanium tetrachloride that takes by weighing is dissolved in deionized water, obtain titanium tetrachloride aqueous solution, dacron after the processing that will take by weighing is immersed in 1～3min in the titanium tetrachloride aqueous solution then, the titanium tetrachloride aqueous solution that is impregnated with dacron is added in the high-temperature high-pressure reaction kettle, and be filled to 60～80% of reactor volume with deionized water, sealing, it is that 110～140 ℃ baking oven is dried 3～6h that the reactor of good seal is put into temperature, and question response finishes the back and takes out dacron.
Step 3: will go up the reacted dacron that obtains of step, and with the bath raio of 1:30～50, with cleaning solution washing 10～20min, use heat, cold water cyclic washing then under 70～90 ℃ of conditions, oven dry or dry naturally obtains the dacron after the modification.Cleaning solution is wherein formed by the soda ash of the solid soap flakes of 2g/L, 2g/L is water-soluble.
Dacron behind the titanium tetrachloride hydrothermal modification is washed and drying (is selected A type washing machine for use according to standard GB/T8629-2001 " textiles test with home washings and drying program ", the 4A washing procedure, A type drying program), and according to standard GB/T18830-2009 " evaluation of ultraviolet resistance of fabric " measure dacron ultraviolet resistance behind the titanium tetrachloride hydrothermal modification.After 30 standard washings, the dacron after the modification is at spectral transmittance T＜4.0% of UVB and UVA wave band, Ultraviolet Protection Factor UPF〉50, can be used as the antiultraviolet product.
According to the dacron antibacterial effect behind standard GB/T20944.2-2007 " the evaluation part 2 of antibacterial textile performance: absorption process " mensuration titanium tetrachloride hydrothermal modification.All more than 95%, titanium tetrachloride modified dacron fabric has antibacterial effect to dacron after the modification to the bacteriostasis rates of staphylococcus aureus (ATCC6538) and Escherichia coli (8099).
Titanium tetrachloride and deionized water usage ratio, hydrothermal temperature and time all affect product crystalline phase, crystallization degree, pattern and particle size.When titanium tetrachloride and deionized water usage ratio are controlled between 1:10～1:100, can obtain the good red schorl phase titanium dioxide of physical and chemical stability, fiber surface coats certain thickness nano-titanium dioxide film, agglomeration can not take place in particle, can not deposit too many nano particle in the solution simultaneously, and combine firmly with fiber; When being higher than 1:10, raw material titanium tetrachloride consumption causes waste too greatly, and nano titanium oxide is many again to be deposited in the solution with Granular forms, and the titanium dioxide that fiber surface adheres to is too thick, and attachment fastness is bad, and nano particle comes off easily in the use; When being lower than 1:100, in the solution remaining titanium dioxide nanoparticle seldom, but the titanium dioxide that fiber surface adheres to is very little, does not form continuous films, antiultraviolet and anti-microbial property can be subjected to obvious influence.Reaction temperature and time mainly influence pattern, the size of the crystallization degree and the crystal of product, and the crystalline phase that generates is also had some influences.Hydrothermal temperature is controlled between 110～140 ℃, can generate sphere, the granularity red schorl phase titanium dioxide particle about 20nm; When being lower than 110 ℃, red schorl phase titanium dioxide be can not generate, antiultraviolet, antibiotic purpose do not reached; When being higher than 140 ℃, the fabric feeling after the processing obviously hardens, and the fabric intensity damage is bigger, has lost serviceability.The hydro-thermal reaction time is controlled between 3～6h, can generate the rutile-phase nano-titanium dioxide film at fiber surface; When being lower than 3h, can influence the crystallization degree of nano titanium oxide, ultraviolet resistance is bad; When being higher than 6h, the titanium dioxide granule of generation can be reunited, and granularity obviously increases, and the surface roughness increase easily causes and comes off.
Fig. 1 is the sem photograph before the dacron titanium tetrachloride hydrothermal modification, Fig. 2 is the sem photograph after adopting the inventive method to dacron titanium tetrachloride hydrothermal modification, Fig. 3 is to before the dacron titanium tetrachloride hydrothermal modification, X-ray diffraction curve after the modification, as can be seen from the figure, unmodified PET fiber surface is very smooth, clean, there are not other attachments to exist, PET fiber surface after the modification has coated the granular material of one deck, roughness obviously increases, particle size does not wait to ten microns from several microns, and can see from the high power electromicroscopic photograph, these fine particles are closely to assemble the second particle that forms by nanometer-size die, crystal grain is spherical in shape, and size is even, and average diameter is about 15nm.Dacron is through the diffraction maximum of titanium dioxide having occurred after the modification, diffraction peak intensity at (110), (101) and (211) crystal face place is stronger, tangible orientation is arranged, the reference standard collection of illustrative plates as can be known, the titanium dioxide nanoparticle that fiber surface coats is the high pure rutile phase structure of crystallization degree.By XRD halfwidth method, according to the Scherrer formula, ask for average grain size D=K λ/(β cos θ), wherein: K=0.89, λ=0.1541nm, β are halfwidth, θ is the Bragg angle.The particle diameter of trying to achieve crystal grain by (110) diffraction maximum is 10.2nm, and the particle diameter of trying to achieve crystal grain according to (101) diffraction maximum is 15.8nm, and average grain diameter is at 13nm, and the result is more approaching with electron microscopic observation.
Embodiment 1
Take by weighing the dacron of 10g and the titanium tetrachloride of 5g respectively.Deionized water and ethanol solution sonic oscillation washing 30min under 50KHz power 100W condition that dacron is 1:1 with 80 ℃ of volume ratios, 60 ℃ of oven dry; Titanium tetrachloride dilutes with deionized water in the ratio of 1:10; Then dacron is immersed in 3min in the titanium tetrachloride solution, adds in the high-temperature high-pressure reaction kettle immediately, and be filled to 80% of reactor volume, the reactor of good seal is put into 110 ℃ baking oven and handled 3h with deionized water; Question response is used the 2g/L soap flakes after finishing, and the 2g/L soda ash solution washs 15min with the 1:30 bath raio under 90 ℃ of conditions, then with 95 ℃ of hot water, cold water cyclic washing, 80 ℃ of oven dry.Fig. 4 is that dacron adopts the forward and backward ultraviolet reflection curve of spectrum of this PROCESS FOR TREATMENT.As can be seen, dacron is through (30 washing backs) after the titanium tetrachloride hydrothermal modification, (it is about 6% that 280～315nm) ultraviolet average absorption abilities have improved, and (315～400nm) ultraviolet average absorption abilities have improved about 30% to the UVA wave band to the UVB wave band.
Wash and dryly (select A type washing machine for use according to the dacron of standard GB/T8629-2001 after the titanium tetrachloride hydrothermal modification, the 4A washing procedure, A type drying program), and according to standard GB/T18830-2009 measure dacron ultraviolet resistance behind the titanium tetrachloride hydrothermal modification.After 30 washings, the dacron after the modification is at the spectral transmittance T=3.8% of UVB and UVA wave band, Ultraviolet Protection Factor UPF=52.According to the dacron antibacterial effect behind standard GB/T20944.2-2007 mensuration titanium tetrachloride hydrothermal modification.Dacron after the modification is 96.4% to the bacteriostasis rate of staphylococcus aureus, is 97.8% to colibacillary bacteriostasis rate, has antibacterial effect.
Embodiment 2
Take by weighing the dacron of 15g and the titanium tetrachloride of 5g respectively.Deionized water and ethanol solution sonic oscillation washing 30min under 50KHz power 100W condition that dacron is 1:1 with 60 ℃ of volume ratios, 60 ℃ of oven dry; Titanium tetrachloride dilutes with deionized water in the ratio of 1:100; Then dacron is immersed in 2min in the titanium tetrachloride solution, adds in the high-temperature high-pressure reaction kettle immediately, and be filled to 70% of reactor volume, the reactor of good seal is put into 140 ℃ baking oven and handled 6h with deionized water; Question response is used the 2g/L soap flakes after finishing, and the 2g/L soda ash solution washs 20min with the 1:40 bath raio under 80 ℃ of conditions, then with 95 ℃ of hot water, cold water cyclic washing, 80 ℃ of oven dry.Fig. 5 is that dacron adopts the forward and backward ultraviolet reflection curve of spectrum of this PROCESS FOR TREATMENT.As can be seen, dacron is through (30 washing backs) after the titanium tetrachloride hydrothermal modification, (it is about 2% that 280～315nm) ultraviolet average absorption abilities have improved, and (315～400nm) ultraviolet average absorption abilities have improved about 12% to the UVA wave band to the UVB wave band.
Wash and dryly (select A type washing machine for use according to the dacron of standard GB/T8629-2001 after the titanium tetrachloride hydrothermal modification, the 4A washing procedure, A type drying program), and according to standard GB/T18830-2009 measure dacron ultraviolet resistance behind the titanium tetrachloride hydrothermal modification.After 30 washings, the dacron after the modification is at the spectral transmittance T=3.6% of UVB and UVA wave band, Ultraviolet Protection Factor UPF=50.According to the dacron antibacterial effect behind standard GB/T20944.2-2007 mensuration titanium tetrachloride hydrothermal modification.Dacron after the modification is 93.9% to the bacteriostasis rate of staphylococcus aureus, is 94.7% to colibacillary bacteriostasis rate, has antibacterial effect.
Embodiment 3
Take by weighing the dacron of 20g and the titanium tetrachloride of 5g respectively.Deionized water and ethanol solution sonic oscillation washing 30min under 50KHz power 100W condition that dacron is 1:1 with 90 ℃ of volume ratios, 60 ℃ of oven dry; Titanium tetrachloride dilutes with deionized water in the ratio of 1:80; Then dacron is immersed in 1min in the titanium tetrachloride solution, adds in the high-temperature high-pressure reaction kettle immediately, and be filled to 60% of reactor volume, the reactor of good seal is put into 120 ℃ baking oven and handled 5h with deionized water; Question response is used the 2g/L soap flakes after finishing, and the 2g/L soda ash solution washs 10min with the 1:50 bath raio under 70 ℃ of conditions, then with 95 ℃ of hot water, cold water cyclic washing, 80 ℃ of oven dry.Fig. 6 is that dacron adopts the forward and backward ultraviolet reflection curve of spectrum of this PROCESS FOR TREATMENT.As can be seen, dacron is through (30 washing backs) after the titanium tetrachloride hydrothermal modification, (it is about 6% that 280～315nm) ultraviolet average absorption abilities have improved, and (315～400nm) ultraviolet average absorption abilities have improved about 30% to the UVA wave band to the UVB wave band.
Wash and dryly (select A type washing machine for use according to the dacron of standard GB/T8629-2001 after the titanium tetrachloride hydrothermal modification, the 4A washing procedure, A type drying program), and according to standard GB/T18830-2009 measure dacron ultraviolet resistance behind the titanium tetrachloride hydrothermal modification.After 30 washings, the dacron after the modification is at the spectral transmittance T=3.5% of UVB and UVA wave band, Ultraviolet Protection Factor UPF=51.According to the dacron antibacterial effect behind standard GB/T20944.2-2007 mensuration titanium tetrachloride hydrothermal modification.Dacron after the modification is 95.2% to the bacteriostasis rate of staphylococcus aureus, is 96.3% to colibacillary bacteriostasis rate, has antibacterial effect.
The present invention adopts titanium tetrachloride the dacron surface to be carried out the method for modification, use titanium tetrachloride under hydrothermal condition directly at polyester fabric fibers area load nano-titanium dioxide film, according to titanium tetrachloride and deionized water consumption, factor such as reaction temperature and time is to the influence of load effect, optimization optimization process technology.Test result shows that the dacron after the modification possesses stronger uvioresistant and anti-microbial property, and washing durability is good.This treatment process safety non-pollution, the production efficiency height, easy and simple to handle, save raw material, not obvious to dacron feel and performance impact such as ventilative.
Claims (2)
1. a method that adopts titanium tetrachloride that modification is carried out on the dacron surface is characterized in that, specifically implements according to following steps:
Step 1: the dacron that will treat modification temperature be under 60～90 ℃ of conditions respectively with deionized water and concentration be 95% absolute ethyl alcohol repeatedly sonic oscillation clean dry for standby;
Step 2: according to mass ratio is dacron and titanium tetrachloride after 2～4:1 takes by weighing the processing that step 1 obtains, according to the volume ratio deionized water: titanium tetrachloride is 1:10～100, the titanium tetrachloride that takes by weighing is dissolved in deionized water, obtain titanium tetrachloride aqueous solution, dacron after the processing that will take by weighing is immersed in 1～3min in the titanium tetrachloride aqueous solution then, the titanium tetrachloride aqueous solution that is impregnated with dacron is added in the high-temperature high-pressure reaction kettle, and be filled to 60～80% of reactor volume with deionized water, sealing, it is that 110～140 ℃ baking oven is dried 3～6h that the reactor of good seal is put into temperature, and question response finishes the back and takes out dacron;
Step 3: will go up the reacted dacron that obtains of step, with the bath raio of 1:30～50, temperature be under 70～90 ℃ of conditions with cleaning solution washing 10～20min, use heat, cold water cyclic washing then, oven dry or dry naturally obtains the dacron after the modification.
2. the method that employing titanium tetrachloride according to claim 1 carries out modification to the dacron surface is characterized in that, the cleaning solution in the described step 3 is formed by the soda ash of the solid soap flakes of 2g/L, 2g/L is water-soluble.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102251389A (en) * | 2011-06-22 | 2011-11-23 | 西安工程大学 | Method for modifying polyester fabric by using butyl titanate |
| CN102277725A (en) * | 2011-06-22 | 2011-12-14 | 西安工程大学 | Method for modifying wool fabric by butyl titanate |
| CN102926187A (en) * | 2012-10-18 | 2013-02-13 | 西安工程大学 | Method for modifying polyester fabric by using magnetic nano iron trioxide |
| CN111636193A (en) * | 2020-06-11 | 2020-09-08 | 南通大学 | Composite functional polyester fabric and finishing method thereof |
| CN111648126A (en) * | 2020-06-11 | 2020-09-11 | 南通大学 | Based on modified nanometer TiO2Multifunctional polyester fabric and finishing method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102251389A (en) * | 2011-06-22 | 2011-11-23 | 西安工程大学 | Method for modifying polyester fabric by using butyl titanate |
| CN102277725A (en) * | 2011-06-22 | 2011-12-14 | 西安工程大学 | Method for modifying wool fabric by butyl titanate |
| CN102277725B (en) * | 2011-06-22 | 2013-01-09 | 西安工程大学 | Method for modifying wool fabric by butyl titanate |
| CN102926187A (en) * | 2012-10-18 | 2013-02-13 | 西安工程大学 | Method for modifying polyester fabric by using magnetic nano iron trioxide |
| CN111636193A (en) * | 2020-06-11 | 2020-09-08 | 南通大学 | Composite functional polyester fabric and finishing method thereof |
| CN111648126A (en) * | 2020-06-11 | 2020-09-11 | 南通大学 | Based on modified nanometer TiO2Multifunctional polyester fabric and finishing method |
| CN111648126B (en) * | 2020-06-11 | 2021-05-14 | 南通大学 | Based on modified nanometer TiO2Multifunctional polyester fabric and finishing method |
| CN111636193B (en) * | 2020-06-11 | 2021-05-14 | 南通大学 | Composite functional polyester fabric and finishing method thereof |
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Application publication date: 20100929 |