CN101363190A - Preparation of gemini type composite colloidal sols and applications thereof in UV-preventing and anti-bacteria finishing - Google Patents
Preparation of gemini type composite colloidal sols and applications thereof in UV-preventing and anti-bacteria finishing Download PDFInfo
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Abstract
The invention discloses a preparation method of Gemini cationic TiO2/SiO2 composite sol and an application method on cotton fabric ultraviolet prevention/antibacterial multifunctional finishing thereof, belonging to the textile chemical technology field. The invention uses the precursors of silicon and titanium, Gemini cationic compound, water, catalyst and solvent to prepare the Gemini cationic TiO2/SiO2 composite sol for the cotton fabric ultraviolet prevention/antibacterial finishing. The composite sol has the advantages of simple process, easy reaction control, high product purity, low cost, environmental protection and energy-saving performance. The particle size is smaller than 10nm. After the finishing, uniform films are formed on fabrics which can endow the fabrics with good performances of shielding ultraviolet rays and resisting bacteria and has no strong effect on the wearability of the fabrics.
Description
Technical field
The invention belongs to technical field of textile chemical engineering, be specifically related to a kind of Gemini type CATION TiO
2/ SiO
2The preparation of complex sol and the application on COTTON FABRIC antiultraviolet/antibiotic composite finishing thereof.
Background technology
Along with improving constantly of rapid development of science and technology and people's living standard, people are tending towards aspects such as comfortable, health and safety to the demand of textiless such as clothes also day.COTTON FABRIC since good and cheap, good hygroscopicity, advantage such as comfortable and easy to wear and extremely people like, but COTTON FABRIC makes its further extensive use run into some challenges to ultraviolet ray and the inferior repellence of microorganism.Therefore, COTTON FABRIC is carried out antiultraviolet and antibiotic finish has certain meaning.
At present, the method of making uvioresistant or antibacterial functions textiles on the textiles that nano material is applied to of studying and using mainly contains two classes both at home and abroad: the one, be spun into method, be about to nano-powder and disperse to be melted in the terylene solution, respin into the method for fiber.This method can realize that nano-powder combines preferably with textiles, but this method complex manufacturing, production difficulty height, and can only be applied to chemical fibre textile, and be not suitable for the natural fabric textiles; The 2nd, finishing method is promptly earlier made anti-ultraviolet finishing liquid or antibiotic finishing solution with described nano-powder, fabric is padded or top finish again, makes function fabric.This method is simple, but since between nano-powder and the textiles for the relation of adhering to, do not have the chemical bond combination, exist that fastness to washing is relatively poor, function can not be lastingly and fabric feeling become of inferior quality shortcoming.And because nano particle has the characteristic of easy reunion, this make nano-powder even dispersion so that prepare stable dressing liquid and all have very big difficulty.
Sol-gel process is a kind of new technology of loomage surface modification.The Nano sol that utilizes sol-gel technology preparing can form the thin and transparent gel mould of one deck at fabric face by methods such as coatings, can effectively improve the fabric face performance.Patent CN1585496A discloses a kind of sol-gel process of utilizing and has prepared the titanium Nano sol is prevented the ultraviolet arrangement to COTTON FABRIC method, use this method can give fabric excellence, lasting uv resistance energy, and very little to the feel and the physical and mechanical properties influence of fabric.Prepared a kind of SiO among the patent CN1631996A
2/ TiO
2Composite oxides ultraviolet light screener, this screener have good dispersive property and UV absorption ability and weatherability, and have avoided the blueing phenomenon in the titanium dioxide application.Patent CN1614133A discloses a kind of TiO 2 sol of organic solvent modification COTTON FABRIC has been prevented the method that ultraviolet is put in order, this method has overcome conventional nano particle and has easily assembled on fabric, easily the weak shortcoming of migration and adhesion has been given play to the distinctive performance of nano particle simultaneously.Prepared a kind of titanium colloidal sol among the CN165473A and be used for COTTON FABRIC is carried out antibiotic finish, the COTTON FABRIC of handling through colloidal sol has excellence, durable antibacterial performance, and has the effect that discharges anion, and the feel and the brute force of fabric had no side effect.Disclose a kind of fiber of antibiotic anti-ultraviolet complex function among the patent CN101187079A, this fiber is with nano-TiO
2, nanometer SiO
2, nano-ZnO and nanoscale AgNO
3As the fiber master batch, make by fusion high speed extrusion spinning, this fiber has well anti-ultraviolet and antibacterial effect.
Summary of the invention
The object of the present invention is to provide a kind of Gemini type complex sol.
Another object of the present invention provides a kind of preparation method of Gemini type complex sol, and this method is selected the cationic compound of Gemini, silicon and titanium precursor body, catalyst, solvent, water for use, can prepare complex sol liquid under room temperature or lower temperature.
A further object of the invention provides the application of a kind of above-mentioned complex sol on the anti-ultraviolet of COTTON FABRIC/antibiotic composite finishing, promptly adopt complex sol dressing liquid of the present invention to fabric being flooded or pads processing, again through heat treatment, Ludox in the dressing liquid forms thin film at fiber surface, there is the titania nanoparticles of anti-ultraviolet effect to have the Gemini CATION of antibacterial action to be anchored in the gel mould some, makes fabric have good antiultraviolet and antibacterial effect with some.
Compare with antibacterial process with traditional antiultraviolet, the present invention has following characteristics:
1. this collosol and gel antiultraviolet/antibiotic composite finishing liquid preparing process is simple, and reaction is easy to control, environmental protection and energy saving;
2. Zhi Bei complex sol particle diameter is little, and the film that forms on fabric is very even, has good shielding ultraviolet rays and antibiotic performance, and little to the feel and the physical and mechanical properties influence of fabric;
3. this collosol and gel prevents that ultraviolet/antiseptic agent is the aquosity fabric dressing liquid, and component is simple, and is easy to use, is applicable to conventional collator and basic technology;
4. particularly this method will prevent that ultraviolet and antibiotic two kinds of arrangements combine, and shorten technological process, save manpower and materials greatly, meet very much the theory requirement of modern industry energy-conserving and environment-protective.
Titanium precursor body involved in the present invention is titanate esters such as tetraethyl titanate, metatitanic acid n-propyl, tetrabutyl titanate, butyl titanate, iso-butyl titanate and isopropyl titanate; Related silicon precursor is esters of silicon acis such as ethyl orthosilicate, positive silicic acid propyl ester, butyl silicate, silicic acid isobutyl ester and isopropyl silicate in the invention.
Gemini cationic compound described in the present invention can be 2-dipropanolamine-two (myristyl alkyl dimethyl ammonium chlorides), dimethylene-two (dodecyl dimethyl ammonium bromide), tetramethylene-two (hexadecyldimethyl benzyl ammonium ammonium chloride), hexa-methylene-two (hexadecyldimethyl benzyl ammonium ammonium bromide) etc.
Catalyst among the present invention can be hydrochloric acid, formic acid, sulfuric acid, nitric acid, acetic acid etc.
Solvent among the present invention can be ethanol, propyl alcohol, isopropyl alcohol, butanols, ethylene glycol etc.
Fabric of the present invention is the fabrics in general on the market, is applicable to that fabric of the present invention mainly contains COTTON FABRIC and BLENDED FABRIC thereof.
The specific embodiment
The present invention will be helped further to understand by following embodiment, but content of the present invention can not be limited.
(1) in three-neck flask, adds solvent 30-42 part, esters of silicon acis 20-38 part, water 15-30 part and Gemini cationic compound 1-5 part successively.(50-600r/min) stirs 2-35min on magnetic stirring apparatus, is that the catalyst of 0.01mol/L is added drop-wise in the above-mentioned mixed liquor with the speed of 20-80drop/min with this understanding with 1-3 part concentration.After being added dropwise to complete, adjust the rotating speed (100-600r/min) of magnetic stirring apparatus, at room temperature continuous stirring 24h promptly obtains a kind of Gemini type cationic colloidal silica.
(2) in three-neck flask, add solvent 30-54 part, titanate esters 15-26 part, water 10-30 part successively.(50-600r/min) stirs 2-35min on magnetic stirring apparatus, is that the catalyst of 0.01mol/L is added drop-wise in the above-mentioned mixed liquor with the speed of 20-80drop/min with this understanding with 5-10 part concentration.After being added dropwise to complete, adjust the rotating speed (100-600r/min) of magnetic stirring apparatus, at room temperature continuous stirring 8h promptly obtains a kind of TiO 2 sol.
(3) get the cationic Ludox of Gemini of 1-20 part, be dissolved in the deionized water of 20-70 part, (50-900r/min) stirs 3-40min on magnetic stirring apparatus, with this understanding the TiO 2 sol that makes of the 5-35 part speed with 10-90drop/min is added drop-wise in the above-mentioned mixed liquor.After being added dropwise to complete, adjust the rotating speed (100-900r/min) of magnetic stirring apparatus, at room temperature continuous stirring 3h promptly obtains a kind of Gemini type CATION TiO
2/ SiO
2The antiultraviolet of colloidal sol/antibiotic composite finishing liquid.
(4) soaking one with this composite finishing liquid by dipping, rolls or two two modes of rolling of soaking are prevented ultraviolet/antibiotic composite finishing to woven fabric, with impregnation method knitted fabric is prevented ultraviolet/antibiotic composite finishing, the concentration of composite finishing liquid is 0.5-5% (o.w.f), treatment temperature is 50-80 ℃, and the processing time is 30-50min.The mode composite finishing liquid concentration of padding is 1-8%, pick-up 60-100%.After arrangement was finished, fabric baked 3-15min at 120-200 ℃ then at 60-80 ℃ of preliminary drying.
(5) method of testing, concrete division is as follows:
1. uv resistance can be tested
Adopt spectrophotometer method to come the ultraviolet (uv) transmission performance of test fabric, adopt ultraviolet ray transmissivity (also claiming transmittance, the ratio of the UV transmitted flux of the UV transmitted flux when referring to sample is arranged during) to be used as the evaluation index of uv resistance energy with no sample.
2. anti-microbial property test
Anti-microbial property is with reference to the AATCC100-2004 standard testing.
3. strength test
Test with reference to GB/T3923.1 1 " textile fabric tensile property part 1: the mensuration galley proof method of ultimate strength and elongation at break ".
4. measuring brightness
WSD-III type whiteness instrument is measured the whiteness of fabric, represents with the Henry whiteness value.
(6) embodiment
Example 1 Gemini type CATION TiO
2/ SiO
2The preparation of complex sol
In three-neck flask, add 1 part of 40 parts of ethanol, 30 parts of ethyl orthosilicates, 27 parts in water and dimethylene-two (hexadecyldimethyl benzyl ammonium ammonium chloride) successively.500r/min stirs 15min on magnetic stirring apparatus, and the hydrochloric acid that is 0.01mol/L with 2 parts of concentration is added drop-wise in the above-mentioned mixed liquor with the speed of 40drop/min with this understanding.After being added dropwise to complete, adjust the rotating speed 500r/min of magnetic stirring apparatus, at room temperature continuous stirring 24h promptly obtains a kind of Gemini type Ludox.
In three-neck flask, add 50 parts of ethanol, 25 parts of butyl titanates, 20 parts in water successively.600r/min stirs 15min on magnetic stirring apparatus, and the hydrochloric acid that is 0.01mol/L with 5 parts of concentration is added drop-wise in the above-mentioned mixed liquor with the speed of 40drop/min with this understanding.After being added dropwise to complete, adjust the rotating speed 500r/min of magnetic stirring apparatus, at room temperature continuous stirring 8h promptly obtains a kind of TiO 2 sol.
Get 15 parts Gemini type cationic colloidal silica, be dissolved in 65 parts the deionized water, 800r/min stirs 3-40min on magnetic stirring apparatus, with this understanding 20 parts the TiO 2 sol that the makes speed with 60drop/min is added drop-wise in the above-mentioned mixed liquor.After being added dropwise to complete, (800r/min, at room temperature continuous stirring 3h promptly obtains a kind of Gemini type CATION TiO to the rotating speed of adjustment magnetic stirring apparatus
2/ SiO
2The antiultraviolet of colloidal sol/antibiotic composite finishing liquid.
Example 2 pure cotton woven fabric infusion process antiultraviolet/antibiotic finishes
Selecting cloth specimen for use is textile plain fabric (20tex * 20tex) through destarch, concise, bleaching.
Concrete technology is as follows:
Get 2g through destarch, concise, the bleaching textile plain fabric (20tex * 20tex), put into Gemini type composite Ti O
2/ SiO
2Handle 60min in the complex sol, the fabric 60 ℃ of oven dry in convection oven with after the arrangement bake 3min again under 150 ℃.
The uv transmittance of the COTTON FABRIC of putting in order through said method approaches 15.5% at the UVA wave band, and the UVB wave band approaches 2.5%, and the UVC wave band then approaches 1%, and promptly fabric has uvioresistant effect preferably; Record cloth specimen staphylococcus aureus and colibacillary bacteriostasis rate are respectively 92.1%, 90.5%, promptly fabric has better anti-bacterial effect.The cloth specimen brute force becomes 753N by 798N before and after handling, and whiteness then becomes 93.25 by 93.89, and promptly this arrangement process is not very big to the brute force and the whiteness influence of fabric.
Example 3 pure cotton woven fabric padding method antiultraviolet/antibiotic finishes
Selecting cloth specimen for use is textile poplin cloth woven fabric (40tex * 40tex) through destarch, concise, bleaching.
Concrete technology is as follows:
Get 2g through destarch, concise, the bleaching textile poplin cloth woven fabric (40tex * 40tex), put into Gemini type composite Ti O
2/ SiO
2Adopt two two modes of rolling of soaking to handle in the complex sol, pick-up is 65%, and the fabric 60 ℃ of oven dry in convection oven with after the arrangement bake 3min again under 150 ℃.
The uv transmittance of the COTTON FABRIC of putting in order through said method approaches 15% at the UVA wave band, and the UVB wave band approaches 2%, and the UVC wave band then approaches 1%, and promptly fabric has uvioresistant effect preferably; Record cloth specimen staphylococcus aureus and colibacillary bacteriostasis rate are respectively 93.1%, 90.5%, promptly fabric has better anti-bacterial effect.The cloth specimen brute force becomes 777N by 812N before and after handling, and whiteness then becomes 92.87 by 93.72.
Example 4 pure cotton knitted fabric infusion process antiultraviolet/antibiotic finishes
The cloth specimen of selecting for use is process destarch, concise, bleached whole cotton combing knitted fabric (27.8tex).
Get 2g and will put into Gemini type composite Ti O through destarch, concise, bleached whole cotton combing knitted fabric (27.8tex)
2/ SiO
2Handle 60min in the complex sol, the fabric 60 ℃ of oven dry in convection oven with after the arrangement bake 3min again under 150 ℃.
The uv transmittance of the COTTON FABRIC of putting in order through said method approaches 15.8% at the UVA wave band, and the UVB wave band approaches 1.6%, and the UVC wave band then approaches 1.2%, and promptly fabric has uvioresistant effect preferably; Record cloth specimen staphylococcus aureus and colibacillary bacteriostasis rate are respectively 96.8%, 95.5%, promptly fabric has preventing ultraviolet effect preferably.The cloth specimen brute force becomes 721N by 754N before and after handling, and whiteness then becomes 93.35 by 93.74, and is less to the brute force and the whiteness influence of fabric.
Claims (10)
1. a complex sol liquid is made up of following material: silicon and titanium precursor body, Gemini cationic compound, water, catalyst and solvent.
2. titanium precursor body involved in the present invention is titanate esters such as tetraethyl titanate, metatitanic acid n-propyl, tetrabutyl titanate, butyl titanate, iso-butyl titanate and isopropyl titanate; Related silicon precursor is esters of silicon acis such as ethyl orthosilicate, positive silicic acid propyl ester, butyl silicate, silicic acid isobutyl ester and isopropyl silicate in the invention.
3. the Gemini cationic compound described in the present invention can be 2-dipropanolamine-two (myristyl alkyl dimethyl ammonium chlorides), dimethylene-two (dodecyl dimethyl ammonium bromide), tetramethylene-two (hexadecyldimethyl benzyl ammonium ammonium chloride), hexa-methylene-two (hexadecyldimethyl benzyl ammonium ammonium bromide) etc.
4. the catalyst among the present invention can be hydrochloric acid, formic acid, sulfuric acid, nitric acid, acetic acid etc.
5. the solvent among the present invention can be ethanol, propyl alcohol, isopropyl alcohol, butanols, ethylene glycol etc.
6. as the preparation method of claims 1 described complex sol liquid, it is characterized in that adopting following method to prepare the cationic Ludox of Gemini: in three-neck flask, to add solvent 30-42 part, esters of silicon acis 20-38 part, water 15-30 part and Gemini cationic compound 1-5 part successively.(50-600r/min) stirs 2-35min on magnetic stirring apparatus, is that the catalyst of 0.01mol/L is added drop-wise in the above-mentioned mixed liquor with the speed of 20-80drop/min with this understanding with 1-3 part concentration.After being added dropwise to complete, adjust the rotating speed (100-600r/min) of magnetic stirring apparatus, at room temperature continuous stirring 24h promptly obtains the cationic Ludox of a kind of Gemini.
7. as the preparation method of claims 1 described complex sol liquid, it is characterized in that adopting following method to prepare TiO 2 sol: in three-neck flask, to add solvent 30-54 part, titanate esters 15-26 part, water 10-30 part successively.(50-600r/min) stirs 2-35min on magnetic stirring apparatus, is that the catalyst of 0.1mol/L is added drop-wise in the above-mentioned mixed liquor with the speed of 20-80drop/min with this understanding with 5-10 part concentration.After being added dropwise to complete, adjust the rotating speed (100-600r/min) of magnetic stirring apparatus, at room temperature continuous stirring 8h promptly obtains a kind of TiO 2 sol.
8. as the preparation method of claims 1 described complex sol liquid, it is characterized in that adopting following method to prepare Gemini type CATION TiO
2/ SiO
2Colloidal sol: get 1-20 part as the cationic Ludox of letter of authorization 7 described Gemini, be dissolved in the deionized water of 20-70 part, (50-900r/min) stirs 3-40min, being added drop-wise in the above-mentioned mixed liquor as the speed of letter of authorization 8 described TiO 2 sols with 10-90drop/min 5-35 part with this understanding on magnetic stirring apparatus.After being added dropwise to complete, adjust the rotating speed (100-900r/min) of magnetic stirring apparatus, at room temperature continuous stirring 3h promptly obtains a kind of Gemini type CATION TiO
2/ SiO
2The antiultraviolet of colloidal sol/antibiotic composite finishing liquid.
9. as claims 1 application of described composite finishing liquid on COTTON FABRIC antiultraviolet/antibiotic composite finishing, it is characterized in that adopting following processing method: cotton fabrics and knitted fabric are carried out antiultraviolet/antibiotic composite finishing by the mode of flooding or pad with this complex sol dressing liquid.The concentration of the mode dressing liquid of dipping is 0.5-5% (o.w.f), and treatment temperature is 50-80 ℃, and the processing time is 30-50min.The mode dressing liquid concentration of padding is 1-8%, pick-up 60-100%.After arrangement was finished, fabric baked 3-15min at 120-200 ℃ then at 60-80 ℃ of preliminary drying.
10. as claims 1 described complex sol dressing liquid, it is characterized in that the fabric that is adapted to is COTTON FABRIC and BLENDED FABRIC thereof.
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| CN102154829B (en) * | 2010-12-20 | 2012-11-07 | 北京服装学院 | Fuzzing, pilling and ultraviolet-prevention finishing agent and preparation method and application |
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| CN102965912A (en) * | 2012-11-20 | 2013-03-13 | 江南大学 | Preparation method of alkaline reaction type silicon-titanium collosol applicable to thermal transfer printing of cotton fabric |
| CN103469557A (en) * | 2013-08-21 | 2013-12-25 | 昆山铁牛衬衫厂 | Method for finishing ultraviolet-proof antibacterial fabric |
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| CN104939388A (en) * | 2015-05-29 | 2015-09-30 | 安徽创荣服装辅料有限公司 | Nanometer shoulder piece |
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| CN108189181A (en) * | 2017-12-29 | 2018-06-22 | 贵州省林业科学研究院 | A kind of preparation method of timber preservative |
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Assignee: Jiangsu Kuangda Automobile Weaving Group Co., Ltd. Assignor: Jiangnan University Contract record no.: 2012320000361 Denomination of invention: Preparation of gemini type composite colloidal sols and applications thereof in UV-preventing and anti-bacteria finishing Granted publication date: 20120229 License type: Exclusive License Open date: 20090211 Record date: 20120330 |
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