CN104233786A - Method for producing silk fabric functionalized by titanium dioxide nanoparticles - Google Patents
Method for producing silk fabric functionalized by titanium dioxide nanoparticles Download PDFInfo
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- CN104233786A CN104233786A CN201410495900.8A CN201410495900A CN104233786A CN 104233786 A CN104233786 A CN 104233786A CN 201410495900 A CN201410495900 A CN 201410495900A CN 104233786 A CN104233786 A CN 104233786A
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Abstract
The invention discloses a method for producing silk fabric functionalized by titanium dioxide nanoparticles. The method comprises the following steps: immersing the silk fabric into a titanium precursor solution, and then putting in boiling deionized water for severely hydrolyzing the titanium precursor solution; forming titanium dioxide nanoparticles in micropores of the inner part of silk through high-temperature hydro-thermal treatment, removing loose substances on the surface through ultrasonic treatment and washing, and drying to obtain the silk fabric containing the titanium dioxide nanoparticles; putting the silk fabric in a silver ion solution to graft silver ions in an ultraviolet environment, and then washing and airing to obtained the silk fabric functionalized by the titanium dioxide nanoparticles. The silk fabric is endowed with an excellent ultraviolet protection capacity and an anti-aging capacity, is good in color and luster and good in wearing comfort and air permeability, and has certain mildew-proof and antibacterial capacities.
Description
Technical field:
The invention belongs to textile material technical field, particularly a kind of production method of silk fabric of titania nanoparticles functionalization.
Background technology:
Be called the silk of fiber queen as far back as first three 4,000 years Christian era just for dress material dress ornament, its all function admirable in style, feel, gloss, intensity and dyeing etc., but have easy yellowing and the shortcoming such as to wear no resistance.Silk fiber is not solid fibers completely, and all there is micropore between fibril arranged side by side and micro-fibril, porosity reaches about 38%.Silk forms primarily of fibroin, and fibroin contains the serine of hydroxyl, and serine is in the regular repeated arrangement of fibroin molecule, so can will functional chemical molecule attached to serine change the physical property of silk fiber and give other functional characters.
Nano titanium oxide self stability is high, colorless and odorless, totally nontoxic, excellent performance, is applied to field of textiles, can gives the effects such as textile fabric uvioresistant, anti-aging, anti-corrosive antibacterial usually through additive process when co-blended spinning and polymerization.
The synthetic method that nano silver antibacterial fabric is conventional mainly contains processbearing astrocyte and adds and fabric post-treatment two kinds of methods, and the good anti-bacterial effect of these two kinds of methods, but poor stability, long-term antibacterial effect is undesirable, and expensive.
Summary of the invention:
The object of this invention is to provide a kind of production method of silk fabric of titania nanoparticles functionalization, the method is by silk fabric and the permanent compound of functional form material, hydrothermal synthesis method is utilized to be entered by titania nanoparticles in the micropore of silk inside, titania nanoparticles is combined with silk fiber and closely becomes an individual system, again with system for overall grafting silver ion, the silk fabric of preparation is permanent possesses the good characteristic of titanium dioxide nano material and the excellent antibacterial of silver ion, obtains multi-functional, high-quality green silk fabric.
Object of the present invention is achieved through the following technical solutions:
A production method for the silk fabric of titania nanoparticles functionalization, comprises the following steps:
(1) immerse in the precursor solution of titanium by silk fabric, 20-30 DEG C leaves standstill, and silk fabric inside is fully infiltrated by the precursor solution of titanium;
(2) silk fabric is taken out from the precursor solution of titanium, remove the precursor solution of the titanium of adsorption, put into the deionized water of 95-100 DEG C, hydrolysis 20-40min, the presoma of the titanium of silk fabric inside is hydrolyzed into unformed titanium dioxide;
(3) silk fabric is taken out from deionized water, put into autoclave, high-temperature water heat treatment 5-7h, make silk fabric inside form the titania nanoparticles of crystal formation;
(4) taken out from autoclave by silk fabric, ultrasonic process removing surface conjunction material loosely, then spend deionized water, 20-30 DEG C of oven dry obtains the silk fabric containing titania nanoparticles.
(5) silk fabric step 4 obtained immerses in silver ion solution, places 2-5min under ultraviolet environments, spends deionized water and dries, obtain the silk fabric of titania nanoparticles functionalization after taking out silk fabric.
Preferred as technique scheme, the presoma of the titanium described in step (1) is the one in tetraethyl titanate, isopropyl titanate, Butyl Phthalate, titanium tetrachloride, titanium sulfate, is especially the one in tetraethyl titanate, isopropyl titanate, Butyl Phthalate.
Preferred as technique scheme, the time of repose described in step (1) is 12-15h.
Preferred as technique scheme, the unformed titanium dioxide described in step (2) is White Flocculus.
Preferred as technique scheme, the axe core of the autoclave described in step (3) is polytetrafluoroethylmaterial material.
Preferred as technique scheme, the temperature of the high temperature described in step (3) is 120-150 DEG C.
Preferred as technique scheme, the titania nanoparticles of the crystal formation described in step (3) is anatase titanium dioxide.
Preferred as technique scheme, the time of the ultrasonic process described in step (4) is 2-5min.
Preferred as technique scheme, the silver ion solution described in step (5) is liquor argenti nitratis ophthalmicus.
Beneficial effect of the present invention is: utilize Hydrothermal Preparation of Nano Titanium Dioxide Materials, can react under relatively low thermal stress conditions, avoids the injury of high temperature to silk fabric.Preferably use the presoma of alcohol titanium salt as titanium of tetraethyl titanate, isopropyl titanate, Butyl Phthalate, high temperature, silver ion and acid condition can be avoided the injury of silk fabric, preserve the primary characteristic of silk fabric as far as possible.Titania nanoparticles is entered in the micropore of silk inside, recycling hydro-thermal method generates titania nanoparticles in silk inside, titania nanoparticles is combined with silk fabric and closely becomes an individual system, by permanent for the good characteristic of titanium dioxide nano material imparting silk fabric.Under ultraviolet environments, promote that grafting is carried out on the surface of silver ion and silk fabric, the adhesion of silver ion and silk is stronger, can improve the long-term antibacterial effect of silk fabric.Silk fabric prepared by the method has fantabulous ultraviolet protection ability, ageing resistance, and the color and luster of fabric is excellent, and comfortableness and the gas permeability of dress are good, has certain antimildew and antibacterial ability.
Detailed description of the invention:
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, and this embodiment only for explaining the present invention, does not form limiting the scope of the present invention.
Embodiment 1:
Silk fabric is immersed in the presoma-tetraethyl titanate solution of titanium, 20 DEG C of standing 12h, after silk fabric inside is fully infiltrated by the precursor solution of titanium, silk fabric is taken out from the precursor solution of titanium, remove the precursor solution of the titanium of adsorption, put into the deionized water of 95 DEG C, hydrolysis 40min, the presoma of the titanium of silk fabric inside is hydrolyzed into the titanium dioxide of unformed White Flocculus;
Silk fabric is taken out from deionized water, put into the autoclave that axe core is polytetrafluoroethylmaterial material, 120 DEG C of hydrothermal treatment consists 7h, silk fabric inside is made to form the titania nanoparticles of anatase titanium dioxide, silk fabric is taken out from autoclave, ultrasonic process 2min, removing surface conjunction material loosely, spend deionized water, 20 DEG C of oven dry obtain the silk fabric containing titania nanoparticles.Silk fabric containing titania nanoparticles is immersed in liquor argenti nitratis ophthalmicus, under ultraviolet environments, places 2min, spend deionized water after taking out silk fabric and dry, obtain the silk fabric of titania nanoparticles functionalization.
The ultraviolet protection coefficient UPF value recording the silk fabric of titania nanoparticles functionalization is 117.4, is 100% to colibacillary bacteriostasis rate, and after washing 30 times, ultraviolet protection coefficient and the loss late to colibacillary bacteriostasis rate are 89.1% and 85.4%.
Embodiment 2:
Silk fabric is immersed in the presoma-isopropyl titanate solution of titanium, 30 DEG C of standing 12h, after silk fabric inside is fully infiltrated by the precursor solution of titanium, silk fabric is taken out from the precursor solution of titanium, remove the precursor solution of the titanium of adsorption, put into the deionized water of 100 DEG C, hydrolysis 20min, the presoma of the titanium of silk fabric inside is hydrolyzed into the titanium dioxide of unformed White Flocculus;
Silk fabric is taken out from deionized water, puts into the autoclave that axe core is polytetrafluoroethylmaterial material, 150 DEG C of hydrothermal treatment consists 7h, make silk fabric inside form the titania nanoparticles of anatase titanium dioxide; Taken out from autoclave by silk fabric, ultrasonic process 5min, removing surface conjunction material loosely, then spend deionized water, 30 DEG C of oven dry obtain the silk fabric containing titania nanoparticles.Silk fabric containing titania nanoparticles is immersed in liquor argenti nitratis ophthalmicus, under ultraviolet environments, places 5min, spend deionized water after taking out silk fabric and dry, obtain the silk fabric of titania nanoparticles functionalization.
The ultraviolet protection coefficient UPF value recording the silk fabric of titania nanoparticles functionalization is 113.4, is 97% to colibacillary bacteriostasis rate, and after washing 30 times, ultraviolet protection coefficient and the loss late to colibacillary bacteriostasis rate are 95.4% and 91.6%.
Embodiment 3:
Silk fabric is immersed in the presoma-Butyl Phthalate solution of titanium, 25 DEG C of standing 14h, after silk fabric inside is fully infiltrated by the precursor solution of titanium, silk fabric is taken out from the precursor solution of titanium, remove the precursor solution of the titanium of adsorption, put into the deionized water of 100 DEG C, hydrolysis 30min, the presoma of the titanium of silk fabric inside is hydrolyzed into the titanium dioxide of unformed White Flocculus;
Silk fabric is taken out from deionized water, puts into the autoclave that axe core is polytetrafluoroethylmaterial material, 130 DEG C of hydrothermal treatment consists 6h, make silk fabric inside form the titania nanoparticles of anatase titanium dioxide; Taken out from autoclave by silk fabric, ultrasonic process 3min, removing surface conjunction material loosely, then spend deionized water, 25 DEG C of oven dry obtain the silk fabric containing titania nanoparticles.Silk fabric containing titania nanoparticles is immersed in liquor argenti nitratis ophthalmicus, under ultraviolet environments, places 3min, spend deionized water after taking out silk fabric and dry, obtain the silk fabric of titania nanoparticles functionalization.
The ultraviolet protection coefficient UPF value recording the silk fabric of titania nanoparticles functionalization is 113.7, is 98% to colibacillary bacteriostasis rate, and after washing 30 times, ultraviolet protection coefficient and the loss late to colibacillary bacteriostasis rate are 95.7% and 92.5%.
Embodiment 4:
Silk fabric is immersed in the presoma-tetraethyl titanate solution of titanium, 20 DEG C of standing 12h, after silk fabric inside is fully infiltrated by the precursor solution of titanium, silk fabric is taken out from the precursor solution of titanium, remove the precursor solution of the titanium of adsorption, put into the deionized water of 95 DEG C, hydrolysis 20min, the presoma of the titanium of silk fabric inside is hydrolyzed into the titanium dioxide of unformed White Flocculus;
Silk fabric is taken out from deionized water, puts into the autoclave that axe core is polytetrafluoroethylmaterial material, 120 DEG C of hydrothermal treatment consists 5h, make silk fabric inside form the titania nanoparticles of anatase titanium dioxide; Taken out from autoclave by silk fabric, ultrasonic process 2min, removing surface conjunction material loosely, then spend deionized water, 20 DEG C of oven dry obtain the silk fabric containing titania nanoparticles.Silk fabric containing titania nanoparticles is immersed in liquor argenti nitratis ophthalmicus, under ultraviolet environments, places 2min, spend deionized water after taking out silk fabric and dry, obtain the silk fabric of titania nanoparticles functionalization.
The ultraviolet protection coefficient UPF value recording the silk fabric of titania nanoparticles functionalization is 109.4, is 97% to colibacillary bacteriostasis rate, and after washing 30 times, ultraviolet protection coefficient and the loss late to colibacillary bacteriostasis rate are 91.8% and 89.6%.
Embodiment 5:
Silk fabric is immersed in the presoma-isopropyl titanate solution of titanium, 30 DEG C of standing 15h, after silk fabric inside is fully infiltrated by the precursor solution of titanium, silk fabric is taken out from the precursor solution of titanium, remove the precursor solution of the titanium of adsorption, put into the deionized water of 100 DEG C, hydrolysis 40min, the presoma of the titanium of silk fabric inside is hydrolyzed into unformed titanium dioxide, is White Flocculus;
Silk fabric is taken out from deionized water, puts into the autoclave that axe core is polytetrafluoroethylmaterial material, 150 DEG C of hydrothermal treatment consists 7h, make silk fabric inside form the titania nanoparticles of anatase titanium dioxide; Taken out from autoclave by silk fabric, ultrasonic process 5min, removing surface conjunction material loosely, then spend deionized water, 30 DEG C of oven dry obtain the silk fabric containing titania nanoparticles.Silk fabric containing titania nanoparticles is immersed in liquor argenti nitratis ophthalmicus, under ultraviolet environments, places 5min, spend deionized water after taking out silk fabric and dry, obtain the silk fabric of titania nanoparticles functionalization.
The ultraviolet protection coefficient UPF value recording the silk fabric of titania nanoparticles functionalization is 118.3, is 100% to colibacillary bacteriostasis rate, and after washing 30 times, ultraviolet protection coefficient and the loss late to colibacillary bacteriostasis rate are 93.1% and 89.4%.
Claims (9)
1. a production method for the silk fabric of titania nanoparticles functionalization, is characterized in that comprising the following steps:
(1) immerse in the precursor solution of titanium by silk fabric, 20-30 DEG C leaves standstill, and silk fabric inside is fully infiltrated by the precursor solution of titanium;
(2) silk fabric is taken out from the precursor solution of titanium, remove the precursor solution of the titanium of adsorption, put into the deionized water of 95-100 DEG C, hydrolysis 20-40min, the presoma of the titanium of silk fabric inside is hydrolyzed into unformed titanium dioxide;
(3) silk fabric is taken out from deionized water, put into autoclave, high-temperature water heat treatment 5-7h, make silk fabric inside form the titania nanoparticles of crystal formation;
(4) taken out from autoclave by silk fabric, ultrasonic process removing surface conjunction material loosely, then spend deionized water, 20-30 DEG C of oven dry obtains the silk fabric containing titania nanoparticles.
(5) silk fabric step 4 obtained immerses in silver ion solution, places 2-5min under ultraviolet environments, spends deionized water and dries, obtain the silk fabric of titania nanoparticles functionalization after taking out silk fabric.
2. the production method of the silk fabric of a kind of titania nanoparticles functionalization according to claim 1, it is characterized in that: the presoma of the titanium described in step (1) is the one in tetraethyl titanate, isopropyl titanate, Butyl Phthalate, titanium tetrachloride, titanium sulfate, is especially the one in tetraethyl titanate, isopropyl titanate, Butyl Phthalate.
3. the production method of the silk fabric of a kind of titania nanoparticles functionalization according to claim 1, is characterized in that: the time of repose described in step (1) is 12-15h.
4. the production method of the silk fabric of a kind of titania nanoparticles functionalization according to claim 1, is characterized in that: the unformed titanium dioxide described in step (2) is White Flocculus.
5. the production method of the silk fabric of a kind of titania nanoparticles functionalization according to claim 1, is characterized in that: the axe core of the autoclave described in step (3) is polytetrafluoroethylmaterial material.
6. the production method of the silk fabric of a kind of titania nanoparticles functionalization according to claim 1, is characterized in that: the temperature of the high temperature described in step (3) is 120-150 DEG C.
7. the production method of the silk fabric of a kind of titania nanoparticles functionalization according to claim 1, is characterized in that: the titania nanoparticles of the crystal formation described in step (3) is anatase titanium dioxide.
8. the production method of the silk fabric of a kind of titania nanoparticles functionalization according to claim 1, is characterized in that: the time of the ultrasonic process described in step (4) is 2-5min.
9. the production method of the silk fabric of a kind of titania nanoparticles functionalization according to claim 1, is characterized in that: the silver ion solution described in step (5) is liquor argenti nitratis ophthalmicus.
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Cited By (4)
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CN105568669A (en) * | 2015-12-31 | 2016-05-11 | 苏州榕绿纳米科技有限公司 | Antibiotic textile and production method thereof |
CN107687088A (en) * | 2017-09-04 | 2018-02-13 | 西南大学 | Conductive silk fabric is prepared with zinc chloride/formic acid solution |
CN109930284A (en) * | 2019-01-21 | 2019-06-25 | 杭州丝绸之路文化艺术有限公司 | The real silk fabric of fungus-resistant extremely preparation method |
CN113737521A (en) * | 2021-09-27 | 2021-12-03 | 溧阳市天目湖农业发展有限公司 | Long-acting antibacterial natural silk fiber and processing technology thereof |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105568669A (en) * | 2015-12-31 | 2016-05-11 | 苏州榕绿纳米科技有限公司 | Antibiotic textile and production method thereof |
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CN107687088A (en) * | 2017-09-04 | 2018-02-13 | 西南大学 | Conductive silk fabric is prepared with zinc chloride/formic acid solution |
CN109930284A (en) * | 2019-01-21 | 2019-06-25 | 杭州丝绸之路文化艺术有限公司 | The real silk fabric of fungus-resistant extremely preparation method |
CN113737521A (en) * | 2021-09-27 | 2021-12-03 | 溧阳市天目湖农业发展有限公司 | Long-acting antibacterial natural silk fiber and processing technology thereof |
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Application publication date: 20141224 |