CN1900410A - Method for preparing fiber with anti-violet and antibiotic property - Google Patents
Method for preparing fiber with anti-violet and antibiotic property Download PDFInfo
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- CN1900410A CN1900410A CN 200610043119 CN200610043119A CN1900410A CN 1900410 A CN1900410 A CN 1900410A CN 200610043119 CN200610043119 CN 200610043119 CN 200610043119 A CN200610043119 A CN 200610043119A CN 1900410 A CN1900410 A CN 1900410A
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Abstract
The present invention provides fiber having persistence uvioresistant mold resistance, belonging to weaving and application area.It contains cotton, ramie, flax, Jute, gambo hemp, cannabis Sativa, Apocynum venetum, hair, tussah silk, mulberry silk, textile fibre, weaving products and methyloic chemical fiber like substance. Said method contains to make fiber carboxy methylation reaction to generate carboxymethyl cellulose, after through carboxymethyl cellulose with butyl titanate hydrolytic reaction to generate chemical bonding nano titanium oxide - carboxymethyl cellulose. Said invention has strong uvioresistant antibiosis ability, lasting action, solving easy desorption shortage of traditional method.
Description
Technical field the present invention relates to the method that a kind of preparation has the fiber of uvioresistant, anti-microbial property, this method is that nano titanium oxide is connected with the mode of cellulose with chemical bond, solved the problem of traditional mode with physical absorption with titanium dioxide deposition existing easy desorption on fiber, the fiber of preparing with this method has good long-acting uvioresistant performance.
The development and use of the current reinforcement bast-fibre of background technology resource have become the common key subjects of paying close attention to of global textile and paper industry, ramie is a kind of native cellulose fibre, gas permeability than cotton fiber Senior Three doubly about, the moisture absorption moisture resistance is good, advantages such as that ramie fabric has is well-pressed, elegant, slim and graceful, nice and cool, ventilative, antibiotic, health care, anticorrosion, fungi-proofing, antimildew function, has the good wearability of wearing, all kinds of health care products of suitable weaving are acknowledged as " king of natural fabric ".Therefore, ramie fabric more and more is subjected to consumer's welcome, especially is subjected to abroad consumer's favor.Gunny products is the valuable cargo of China foreign exchange earning, and China has 90% ramie product to export to western countries approximately, therefore, exploitation, the processing of ramee is had very important meaning.And it is at present also less about the bibliographical information of the exploitation of ramee and textiles thereof.
Current social economy high speed development has also brought the destruction of serious problems, particularly ozone layer such as environmental pollution to be on the rise, and the ultraviolet intensity that arrives ground significantly increases, and ultraviolet ray is also increasing to the injury of human body.Therefore, how to solve ultraviolet injury and become our problem demanding prompt solution.Because nano titanium oxide has good uvioresistant, photocatalysis, anti-microbial property, the additive that is widely used in fiber and fabric recently is to increase uvioresistant, the anti-microbial property of fabric.But generally adopt at present nano titanium oxide is added in fiber or the fabric in the mode of physical deposition, titanium dioxide and fiber or fabric are that the mode by physical absorption combines, and therefore certainly exist the problem of the easy desorption of titanium dioxide in fiber or the fabric.And we carry out modification generation carboxymethyl cellulose earlier with the ramee element, generate the carboxymethyl cellulose that bonding has nano titanium oxide with carboxymethyl cellulose and butyl titanate by slow hydrolysis again.Thereby titanium dioxide is connected nanometer with the mode of fiber with chemical bond,, has solved the problem of the existing easy desorption of mode of traditional physical deposition in conjunction with firmly, lastingly.This method is not seen bibliographical information so far as yet.
Summary of the invention the present invention aims to provide a kind of fiber with persistence uvioresistant, anti-microbial property, comprising: cotton, ramie, flax, jute, bluish dogbane, hemp, bluish dogbane, hair, press for extracting juice silk, mulberry silk, textile fabric, textile fabrics and the chemical fibre class material that contains carboxyl.Different with the preparation method of general uvioresistant, anti-bacterial fibre, this method is earlier fiber to be carried out carboxymethylation reaction to generate carboxymethyl cellulose, generates nano titanium oxide-carboxymethyl cellulose with chemical bonding by slow hydrolysis with carboxymethyl cellulose and butyl titanate in the presence of micro-moisture afterwards.Realized that nano titanium oxide is connected with the mode of fiber with chemical bond.Originally studies show that: the nano titanium oxide-ramee carboxymethyl cellulose with chemical bonding has not only acted on the intrinsic premium properties of ramee, and have stronger uvioresistant, an antibacterial ability, in addition, nano titanium oxide combines firmly, acts on lasting with fiber, fundamentally solved the defective that adopts the existing easy desorption of conventional method.
Description of drawings: figure the-1st, the infrared spectrogram of ramee and carboxymethyl cellulose; Figure the-2nd, the infrared spectrogram of carboxymethyl cellulose and nano-titanium dioxide modified carboxymethyl cellulose; Figure the-3rd, nano-titanium dioxide modified carboxymethyl cellulose-spherical distribution sem photograph; Figure the-4th, nano-titanium dioxide modified carboxymethyl cellulose-covering shape sem photograph; Figure the-5th, the UV, visible light near infrared light spectrogram of nano-titanium dioxide modified carboxymethyl cellulose.
The performance of specific embodiment implementation procedure of the present invention and material is described in detail by following examples:
Embodiment one: (preliminary treatment of ramee element)
Because ramee has higher degree of crystallinity, must carry out activation processing before reacting, so that the carrying out of reaction and the raising of the extent of reaction.The pre-treatment reagent that is used for ramee among the present invention has sodium hydroxide solution, dimethyl sulfoxide (DMSO) etc.The both available usual method of processing method (stirring under the uniform temperature), the method for available sonicated again.
A certain amount of ramee joined in 30% the sodium hydroxide solution, add a spot of dimethyl sulfoxide (DMSO) again, at room temperature stir 10～20h or ultrasonic reaction 1～2h at room temperature, can prepare alkali cellulose, solution is kept in order to next step use.
Embodiment two: (preparation of ramee carboxymethyl cellulose)
In the above-mentioned alkali cellulose solution for preparing, add a certain amount of sodium chloroacetate and a certain amount of catalyst at 40～80 ℃ of following ultrasonic reaction 2h.Stop to react the back and with sulfuric acid the pH value of solution is transferred to 2～3, usefulness absolute ethyl alcohol, distilled water promptly get the ramee carboxymethyl cellulose through filtering and washing repeatedly at last.Carry out the substitution value test of sample at last.
Embodiment three: (influence of catalyst)
In order to improve the substitution value of reaction, in this step reaction, need to add appropriate amount of catalysts, these catalyst can be 4-dimethylamino pyridine (DMAP), Dodecyl trimethyl ammonium chloride, softex kw, KI, n-formyl sarcolysine base pyrrolidones etc.Experiment shows: add appropriate amount of catalysts and can improve the substitution value of reaction in course of reaction.
Embodiment four: (ultrasonic influence to preparation carboxymethyl cellulose result)
Because at a large amount of hydrogen bonds, therefore have higher degree of crystallinity at the intermolecular and molecular memory of ramee element, the interior hydroxyl of crystal region has all formed hydrogen bond, only in the amorphous region, part of hydroxyl does not form hydrogen bond.Usually, chemical reagent can only enter in the amorphous region and hydroxyl reaction, reacts with fiber and can not enter in the crystal region.Therefore before carrying out the ramee modification, at first to carry out preliminary treatment,, make more hydroxyl be " released " out, could improve cellulosic modified effect like this to destroy the hydrogen bond that associates in its crystal region to it.Because ultrasonication has special effect, in the preprocessing process of fiber, introduce the ultrasonic hydrogen bond and the degree of orientation that can destroy in the fiber macromolecular structure, reduce cellulosic degree of crystallinity, help reactant molecule to enter fibre structure inside and react, thereby improve the substitution value of reaction.Ultrasonication simultaneously can accelerated reaction thing molecule motion, improve reaction rate.
In order to improve the substitution value of fiber carboxymethylation reaction, make reaction evenly simultaneously, therefore when carrying out carboxymethylation reaction, in the presence of ultrasonic, react 1～2h.
Embodiment five: (water treatment of ramee carboxymethyl cellulose)
Take by weighing a certain amount of above-mentioned carboxymethyl cellulose for preparing and under different condition, carry out water treatment, to change the moisture in the fiber.Experimental result shows: moisture is seldom the time in the fiber after handling, and fiber surface does not generate titanium dioxide, smooth surface behind late phase reaction.When containing micro-moisture in the fiber, though the sample after the processing generates titanium dioxide in the late phase reaction rear surface, the content of titanium dioxide is very low, and titanium dioxide distributes also inhomogeneous at fiber surface in addition.And when having only sample after handling to contain amount of water, a large amount of nanoscale coverings and spherical tio2 are just contained in the surface of fiber after reaction, are evenly distributed and dispersed better.But moisture more for a long time in the sample after handling, and the titanium dioxide that generates at reacted fiber surface mostly is the big block of reunion, and skewness and content are lower.
Embodiment six: (preparation of nano-titanium dioxide modified ramee)
After under the room temperature carboxymethyl cellulose being carried out water treatment a period of time, put into clean beaker, add a certain amount of absolute ethyl alcohol then respectively, DMSO and a certain amount of butyl titanate.Ultrasonic reaction at room temperature after reactant mixes.Place a period of time in air ultrasonic end back.Use absolute ethyl alcohol, distilled water is filtering and washing repeatedly, and is dry in baking oven afterwards, promptly makes the carboxymethyl cellulose after nano-titanium dioxide modified.
Embodiment seven: (influence of butyl titanate concentration)
The concentration of butyl titanate is under all constant situation of other amount of substances (being that absolute ethyl alcohol and DMSO are constant volume), realize by the volume that changes butyl titanate, different butyl titanate concentration not only can influence the content of titanium dioxide in the fiber, and can influence the pattern and the distribution situation of the titanium dioxide of fiber surface.Experiment shows that when butyl titanate concentration is comparatively moderate the titanium dioxide of fiber surface exists with nanometer covering and spheroidal particle dual mode.Nano-titania particle is evenly distributed at fiber surface, and particle diameter is approximately 200nm.
Embodiment eight: (ultrasonic to preparing the influence of nano-titanium dioxide modified ramee)
Because ultrasonication has dispersion effect preferably, therefore in the process of the nano-titanium dioxide modified ramee of preparation, introduce ultrasonication, the nano titanium oxide of generation is evenly distributed at cellulose surface, the nano-titania particle that adopts this method to prepare simultaneously is better dispersed, particle diameter is even, and diameter is approximately 200nm.
Embodiment nine: (the UV, visible light near infrared absorption of nano-titanium dioxide modified ramee)
The nano-titanium dioxide modified ramee that adopts method for preparing is carried out the test of UV, visible light near infrared spectrum, and figure-5 is its test result.As seen from the figure: the fiber after nano-titanium dioxide modified promptly has strong absorption to ultraviolet light at the 385nm place.So adopt the fiber after this method modification to have stronger uvioresistant performance.
Claims (13)
1. a nanometer uvioresistant, antibiotic multifunction fiber, it has good uvioresistant performance, has antibiotic, mildew-resistant, deodorization, accumulation of heat, function such as nice and cool, ventilative simultaneously.
2. nanometer uvioresistant according to claim 1, antibiotic multifunction fiber preparation method are applicable to cotton, ramie, flax, jute, bluish dogbane, hemp, bluish dogbane, hair, press for extracting juice silk, mulberry silk, textile fabric, textile fabrics and the chemical fibre class material that contains carboxyl.
3. nanometer uvioresistant multifunctional fibre according to claim 1 is characterized in that containing in the above-mentioned fiber nano lamellar and pelletiod nano titanium oxide uvioresistant, antibiotic multifunction powder, and is dispersed in the inside and the top layer of fiber.
4. nanometer uvioresistant according to claim 1, its titanium dioxide of antibiotic multifunction fiber and carboxymethyl cellulose are with the mode bonding of chemical bond, and the existing way of the titanium dioxide of fiber surface is existing to be had with chemical bonding again with physical absorption.
5. be meant unformed nano titanium oxide according to claim 2 or the described nano inorganic uvioresistant of claim 3, antibiotic multifunction powder.
6. be nanometer covering or nanometer particle according to claim 2 or the multi-functional powder of the antibiotic uvioresistant of the described nano titanium oxide inorganic of claim 3.
7. have uvioresistant and function such as antibiotic according to claim 2 or the described nano-titanium dioxide powder of claim 3.
8. the multi-functional ramee of nanometer uvioresistant according to claim 1 is characterized in that indication is multi-functional to generate nano titanium oxide multifunctional inorganic uvioresistant, antibiotic multifunction covering and Nano microsphere by slow hydrolysis by ramie carboxymethyl cellulose and butyl titanate in the presence of micro-moisture and realize.
9. ramie carboxymethyl cellulose according to claim 7 and the reaction of butyl titanate in the presence of micro-moisture are to implement under ultrasound condition by adding dimethyl sulfoxide (DMSO) in the carboxymethyl cellulose that will contain a certain amount of moisture.
10. ramie carboxymethyl cellulose according to claim 3 reacts ramee and sodium chloroacetate to generation in the presence of catalyst.
11. the preparation of ramie carboxymethyl cellulose according to claim 9 is at first with the ramee sodium hydroxide solution, dimethyl sulfoxide (DMSO), under ultrasound condition, carry out swelling pretreatment, in this solution, add afterwards sodium chloroacetate and catalyst at a certain temperature (40～80 ℃) realize.
12. the catalyst of preparation ramie carboxymethyl cellulose according to claim 10 comprises: 4-dimethylamino pyridine (DMAP), Dodecyl trimethyl ammonium chloride, softex kw, KI, n-formyl sarcolysine base pyrrolidones etc.
13 catalyst according to claim 12 can improve the substitution value of fiber carboxymethylation reaction preferably.
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| JP2010077411A (en) * | 2008-08-27 | 2010-04-08 | Sanyo Chem Ind Ltd | Method for producing alkyl-etherified carboxyalkyl cellulose |
| CN101187164B (en) * | 2007-11-28 | 2010-06-09 | 南通大学 | Anti-creasing anti-bacterial anti-ultraviolet composite function silk fabric and its preparation method |
| CN101974858A (en) * | 2010-09-29 | 2011-02-16 | 江苏阳光股份有限公司 | Method for producing cold-feeling deep-color worsted fabrics |
| CN101215780B (en) * | 2007-12-27 | 2012-01-18 | 浙江嘉得莱有限公司 | Pure natural ultra-violet radiation resisting finishing method for knitting plus material |
| CN101724929B (en) * | 2009-11-02 | 2012-05-23 | 大连工业大学 | Method for preparing cellulose/nanometer titanium dioxide blending material in ionic liquid solvent |
| CN102691203A (en) * | 2012-06-15 | 2012-09-26 | 南通大学 | Preparation method of antibacterial and anti-ultraviolet fiber/fabric loaded with nano-titania |
| CN102899884A (en) * | 2012-10-18 | 2013-01-30 | 西安工程大学 | Nanometer titanium dioxide cotton fiber modifying method with improved dyeing property and attachment firmness |
| CN103121712A (en) * | 2013-03-06 | 2013-05-29 | 东北林业大学 | Method for preparation of super long fibrous titanium dioxide by taking cellulosic fibers as template |
| CN103437145A (en) * | 2012-06-15 | 2013-12-11 | 南通大学 | Preparation method of antibacterial and ultraviolet-resistant fabric based on nano titanium dioxide |
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| CN105413753A (en) * | 2015-11-05 | 2016-03-23 | 浙江理工大学 | Preparation method of bast fiber-carried titanium dioxide composite material powder |
| CN105820588A (en) * | 2016-04-20 | 2016-08-03 | 吴江福汇缘家纺有限公司 | Composite silk textile material and preparation method thereof |
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- 2006-07-07 CN CN 200610043119 patent/CN1900410A/en active Pending
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| CN102691203B (en) * | 2012-06-15 | 2013-12-18 | 南通大学 | Preparation method of antibacterial and anti-ultraviolet fiber/fabric loaded with nano-titania |
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| CN102899884B (en) * | 2012-10-18 | 2014-07-02 | 西安工程大学 | Nanometer titanium dioxide cotton fiber modifying method with improved dyeing property and attachment firmness |
| CN103121712A (en) * | 2013-03-06 | 2013-05-29 | 东北林业大学 | Method for preparation of super long fibrous titanium dioxide by taking cellulosic fibers as template |
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