CN104562658B - Amino acid nano-silver modified finishing agent as well as preparation method of finishing agent and modified fishing shell fabric - Google Patents
Amino acid nano-silver modified finishing agent as well as preparation method of finishing agent and modified fishing shell fabric Download PDFInfo
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- CN104562658B CN104562658B CN201510030750.8A CN201510030750A CN104562658B CN 104562658 B CN104562658 B CN 104562658B CN 201510030750 A CN201510030750 A CN 201510030750A CN 104562658 B CN104562658 B CN 104562658B
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Abstract
The invention provides an amino acid nano-silver modified finishing agent as well as a preparation method of the finishing agent and a modified fishing shell fabric. The amino acid nano-silver modified finishing agent is prepared by mixing a silver solution with an amino acid uniformly mixed solution and stirring the mixture for 30-45 minutes at 95-100 DEG C. The amino acid uniformly mixed solution is prepared by mixing an amino acid aqueous solution, a crosslinking agent and a surfactant. Fibers or a fabric of the fibers are dipped and rolled twice, roasted, washed and dried, so that the crease resistance, shrink resistance, the dye-uptake of the dye and the like of the modified finishing shell fabric are obviously improved and enhanced. The amino acid nano-silver modified finishing agent further has the technical advantages of simplified steps, environment-friendly process, closeness to nature and no pollution and short time.
Description
Technical field
Present patent application refers to modification agent and the preparation method of modification agent of fiber and fabric thereof,
Functional fiber that fiber or the collated modification of its fabric obtain or its fabric.
Background technology
Technical research shows, because nanometer silver has the highest specific surface area and surface activity, process based prediction model is stable,
There is superpower sterilization, bacteriostatic activity.Based on this, fiber or its fabric are implemented silver ion modified, make silver ion attachment combine
On cotton fiber body, making cotton fiber have anti-microbial property, this type of fabric-modifying, finishing technique have been seen in relevant public technology,
But these modification technologies only obtain single antibacterial functions, and also with some other technical problem.As, Chinese patent
Technical scheme disclosed in CN201320262131, first cotton fiber is used Methacrylamide grafting to process, by poly-first by scheme
Base acrylamide molecules is graft, the electron rich group amido link in its structure again with silver ion coordination, improve cotton fine
The dimension adsorption to silver ion, it is thus achieved that there is the modified cotton fiber of anti-microbial property.It is single that this programme equally exists modified function
Technical deficiency, and also cotton fiber is implemented pretreatment, a whole set of modified technique is relatively complicated, it addition, record according to its scheme,
Its water-fastness ability is poor, and the modified silver content reserved after cotton fiber washing is only original 75.23%.
Nanometer silver be by reducing agent reduction prepare, the reducing agent that prior art is generally selected include sodium borohydride,
Hydrazine hydrate, glucose, ascorbic acid, sodium hypophosphite, sodium citrate etc., these reducing agent compositions of sodium borohydride, hydrazine hydrate exist
A certain degree of toxicity and carcinogenecity, have potentially hazardous to human body, other organism and environment.With glucose, ascorbic acid
The nanometer silver prepared Deng reduction only obtains antibacterial functions in terms of the finishing functions of fabric, and reducing agent rises not in the fabric arranged
To function affect.
The development consumption demand to be catered to of technology and lead consumption guidance.Along with people to harmony between man and nature relation, from
So the understanding of bound pair Anthroposphere deepens continuously, and is incorporated on fiber by natural materials composition, produces, strengthens, extends and supplement
Beneficial functions, removes, converts and weaken unfavorable factor, is allowed to present the New function getting close to human body or other organism, is weaving
The development trend for the treatment of technology.
Wherein, a kind of natural soluble bio-based materials aminoacid, with its biocompatibility, affinity, containing sky
Right Moisture factor, has the effect preventing skin aging, suppression melanin from generating, and safe and nontoxic natural quality, in recent years
Increasingly to be attracted attention by people.If fabric is implemented amino-acid modified arrangement, can effectively protect the moisture in fiber horny layer,
Play the effect of Glycerin, make skin persistently keep delicate, gloss and elasticity, as skin protection adjustment of judogi fabric, should
For underclothes, such as underwear, shirt, bedding etc., show good in ecological environment-friendly type Final finishing technology is applied
Application prospect.
Aminoacid has manifested at the finishing technique of cellulose base fiber fabric in prior art.Li Shaoquan etc. are " cotton
The preparation of the adsorbable material of fabric aminoacid and sign thereof " literary composition proposes the bafta to the most carboxylated modification implement sericin ammonia
The modification technology of base acid adsorption treatment.Though this technology completes the modification to cotton fiber of the sericin aminoacid, modification is knitted
The hydroscopicity of thing improves a lot, but finds that modified fabric exists the technical problem that washing fastness is poor simultaneously, this be by
Adsorbing for ionic bond between carboxyl on amino acid whose amino and crafted cotton fibers, physical bond power is weak to be caused, it addition, change
Property bafta fracture strength mechanical performance and whiteness all in significantly declining, Boardy Feeling, comfort level is poor, its technical scheme another lead
Wanting technological deficiency is to also need to before modified process cotton fiber is implemented carboxylated modified pretreatment, complex process, operation harmony length, effect
Rate is low.
Chinese patent CN 200710049287 is open describes a technical side amino-acid modified to synthetic fibers enforcement
Case, in its scheme by aminoacid graft copolymerization, be blended and enter in spinning solution in synthetic fiber material strand, the fibre spinned
Dimension silk material needs shaped process, prepares a kind of containing amino acid whose profiled filament, and aminoacid therein is changed by protein
?.The copolymerization of aminoacid and synthetic fibers, being blended in finished fiber, overwhelming majority aminoacid merge and are distributed in fiber
Portion, can the most limited with contact skin, cause amino acid health function to be difficult to comprehensively and given full play to.
In sum, prior art generally exists that modified function is single, Function is limited, whole set process method is returned naturally
Genus degraded performance, the multiple technologies problem that operation is loaded down with trivial details and fabric self-technique performance is the most undesirable.
Summary of the invention
The goal of the invention of present patent application is to provide a kind of fiber more leveling off to natural attribute and environmental requirement
Modifies nanometer silver preparation method, the most compatible the most affine attribute of aminoacid, it is achieved there is multiple modified function and modified work
Skill environmental protection, get close to nature, the amino acid nano-silver modification agent simplifying, being effectively improved the multinomial technical specification of product and preparation thereof
Method and modification fabric.
The amino acid nano-silver modification agent technical scheme that present patent application provides, its main technical content is:
A kind of amino acid nano-silver modification agent, this modification agent is mixed by 1:1 volume ratio by silver solution and the equal miscible fluid of aminoacid
Closing, prepare simultaneously after stirring 30 ~ 45 minutes at a temperature of 95 ~ 100 DEG C, described silver-colored solution is 0.01 ~ 0.05g/L mass concentration
The silver nitrate aqueous solution of scope, the equal miscible fluid of described aminoacid is dividing of amino acid solution, cross-linking agent and surfactant
Dissipating homogeneous mixture solotion, the mass concentration of amino acid solution therein is 20 ~ 60 g/L, and it is sweet that cross-linking agent selects fatty alcohol to shrink
Oil one of ether or polybasic carboxylic acid, mass concentration is 20 ~ 60 g/L, and surfactant is fatty alcohol-polyoxyethylene ether, its quality
Concentration is 2 ~ 6 g/L.
Present patent application is also provided with the preparation method technical scheme of described amino acid nano-silver modification agent, should
Method is: the equal miscible fluid of aminoacid is mixed by 1:1 volume ratio with silver solution, stirs 30 ~ 45 points at a temperature of 95 ~ 100 DEG C simultaneously
Clock, prepares, wherein, the described silver nitrate aqueous solution that silver-colored solution is 0.01 ~ 0.05g/L mass concentration scope, described amino
Acid all miscible fluids are the mixed solutions that is uniformly dispersed of amino acid solution, cross-linking agent and surfactant, amino sour water therein
The mass concentration of solution is 20 ~ 60 g/L, and cross-linking agent selects one of fatty alcohol glycidyl ether or polybasic carboxylic acid, mass concentration
Being 20 ~ 60 g/L, surfactant is fatty alcohol-polyoxyethylene ether, and its mass concentration is 2 ~ 6 g/L.
In above-mentioned technical scheme, described fatty alcohol glycidyl ether is hexylene glycol glycidyl ether, butanediol two
In glycidyl ether, propylene glycol diglycidylether, Ethylene glycol diglycidyl ether one of arbitrarily.
In above-mentioned technical scheme, described polybasic carboxylic acid be in BTCA, citric acid, poly arbitrarily it
One.
In above-mentioned technical scheme, described surfactant is to appoint in Span-80, Tween80, JFC, paregal O
One of meaning.
In above-mentioned technical scheme, described amino acid solution selects the lysine water-soluble with good cost performance
In the aqueous solutions such as liquid, glutamic acid aqueous solution or methionine any one.
Present patent application additionally provides applies changing of described amino acid nano-silver modification agent modification acquisition
Property arrange fabric, corpus fibrosum alleged below or corpus fibrosum fabric be cotton fiber, viscose fiber, tencel fiber, Modal fibre,
Bamboo fibre, flaxen fiber or its fabric.The modification method that the present patent application provides is: corpus fibrosum or the leaching of corpus fibrosum fabric
Entering in amino acid nano-silver modification agent, its bath raio is 1: 30, two rolls through two leachings, every time dipping 15 minutes, liquid carrying rate is 70 ~
90%, by preliminary drying 5 minutes in 40 ~ 80 DEG C of temperature, then bake 3 minutes through 80 ~ 160 DEG C of temperature, be washed to neutrality, drying.
Amino acid nano-silver modification agent disclosed in present patent application, using aminoacid as reducing agent reduced nano
It is introduced into while silver in modification agent, obtains the amino-acid modified finisher solution containing nanometer silver, the particle diameter of nanometer silver
Generally less than 30nm, it is applied to the modification of fiber or its fabric, makes fiber or its fabric face uniformly be fixed with nanometer
Silver and the aminoacid of covalent cross-linking, shown in Fig. 2 is the modification agent modification fabric with lysine as reducing agent, and it is fine
With cross-linking agent and the micro structure of the covalent cross-linking of lysine between cellulose fiber, modified fiber or its fabric is made to be provided simultaneously with
Antibacterial and moisturizing, lead the multiple modified function of skin skin-protection and health-care wet, close, change existing modification technology modified function single
Technical problem, and have and adsorb more by force set with corpus fibrosum, the technological merit that its fastness to washing is greatly improved, overcome existing skill
The technical problem that anti-microbial property is undesirable, fastness to washing is poor that art exists, the fabric after arrangement is after 50 times are washed, to large intestine bar
The bacteriostasis rate of bacterium and staphylococcus aureus the most all can reach more than 95%；The technical program overcome the most simultaneously include cotton fiber,
Viscose fiber, tencel fiber, Modal fibre, bamboo fibre, flaxen fiber or its fabric interior existence easily wrinkle, easily shrink,
Technical problem, modified fiber or its fabrics such as dyestuff dye-uptake is undesirable, crease-resistant, shrink, Dye up-take etc. are technical
Index can be significantly improved and improve, creasy recovery angle improves more than 50 °, and the dye-uptake of dyestuff improves more than 5%, to greatly
The bacteriostasis rate of enterobacteria and staphylococcus aureus reaches more than 99%, makes modified fabric health, comfortableness and attractive in appearance more meets
The use demand of affine human body or other organism.Modification agent preparation method disclosed in the technical program and method of modifying tool
Having operation simplification, technique environmental protection, get close to the technological merit that nature is pollution-free, the used time is short, process cost is low, added value of product is high.
Accompanying drawing explanation
Fig. 1 is dyeing curve chart.
Fig. 2 is cross-linking agent and aminoacid and the micro state schematic diagram of cellulose fibre covalent cross-linking, and waveform therein is long
Shown in curve is cellulose fibre, by crosslinking agent B TCA and lysine LYS covalent cross-linking between two cellulose fibre macromole,
Stain between two cellulose fibre macromole is the nanometer silver of uniformly attachment.
Detailed description of the invention
The technology contents of the present patent application will be illustrated in detail by way of the following examples below.Wherein, also can by viscose fiber,
Tencel fiber, Modal fibre, bamboo fibre, flaxen fiber or its fabric replace the cotton fiber in each embodiment or its fabric,
Effect is identical；Described surfactant, also can be replaced in embodiment by the Span-80 of same apoplexy due to endogenous wind, JFC, paregal O
Tween80, effect is the most identical.
Embodiment 1
Step one, preparation amino acid nano-silver modification agent:
Silver solution be mass concentration be the silver nitrate aqueous solution of 0.01g/L；
The equal miscible fluid of aminoacid is the dispersed mixed solution of following component, is the amino of 20g/L including mass concentration
Aqueous acid, including the hexylene glycol glycidyl ether crosslinking agent that mass concentration is 20g/L, is 2g/L's including mass concentration
Tween-80 surfactant；For the consideration of one-tenth present aspect, amino acid solution can be selected for the most dominant bad ammonia of cost performance
The aqueous solutions such as acid, glutamic acid, methionine；
Silver solution miscible fluid equal with aminoacid is mixed by the volume ratio of 1: 1, and under 95 DEG C of temperature conditionss, mixing speed is the lowest
In 200 revs/min, through 30 minutes, prepare amino acid nano-silver modification agent.
The modification method of step 2, cotton fiber or its fabric:
Cotton fiber or its fabric being immersed in amino acid nano-silver modification agent, its bath raio is 1: 30, rolls through two leachings two,
Impregnating 15 minutes under room temperature, executing roll compacting power is 0.9kg/cm every time2, liquid carrying rate is 70%, and it is placed in baking oven, in 40 DEG C of temperature
Degree preliminary drying 5 minutes, bakes 3 minutes in 80 DEG C of temperature, dries, obtain modification after being washed to neutrality at a temperature of 40 DEG C
Fabric.
Embodiment 2
Step one, preparation amino acid nano-silver modification agent
Silver solution be mass concentration be the silver nitrate aqueous solution of 0.03g/L；
The equal miscible fluid of aminoacid is the dispersed mixed solution of following component: include the amino that mass concentration is 40g/L
Aqueous acid, including the butanetetra-carboxylic acid cross-linking agent that mass concentration is 40g/L, including the Tween-80 surface that mass concentration is 4g/L
Activating agent.Wherein, for the consideration of one-tenth present aspect, amino acid solution can be selected for the more dominant lysine of cost performance, paddy ammonia
The aqueous solutions such as acid, methionine；
Silver solution miscible fluid equal with aminoacid is mixed by the volume ratio of 1: 1, is heated to 100 DEG C, strong stirring 30 minutes, its
Mixing speed is not less than 200 revs/min, prepares amino acid nano-silver modification liquid.
The modification method of step 2, cotton fiber or its fabric
Immersing in amino acid nano-silver modification liquid by cotton fiber or its fabric, its bath raio 1: 30, through two leachings under room temperature
Two roll, every time dipping 15 minutes, and draught pressure is 0.9kg/cm2, liquid carrying rate is 70%, puts in baking oven 80 DEG C of preliminary dryings 5 minutes, then
Bake at a temperature of 160 DEG C 3 minutes, be washed to after neutrality in 80 DEG C of drying, obtain modification product.
Embodiment 3
Step one, preparation amino acid nano-silver modification agent
Silver solution be mass concentration be the silver nitrate aqueous solution of 0.05g/L；
The equal miscible fluid of aminoacid is the dispersed mixed solution of following raw material: include the amino that mass concentration is 60g/L
Aqueous acid, including the butanetetra-carboxylic acid cross-linking agent that mass concentration is 60g/L, including the Tween-80 surface that mass concentration is 6g/L
Activating agent；Wherein for the consideration of one-tenth present aspect, amino acid solution can be selected for the more dominant lysine of cost performance, paddy ammonia
The aqueous solutions such as acid, methionine；
Silver solution miscible fluid equal with aminoacid is mixed by the volume ratio of 1: 1, and under 95 DEG C of temperature conditionss, mixing speed is the lowest
In 200 revs/min, through 30 minutes, prepare amino acid nano-silver modification agent.
The modification method of step 2, cotton fiber or its fabric
Immersing in amino acid nano-silver modification agent by cotton fiber or its fabric, its bath raio 1: 30, through two leachings under room temperature
Two roll, every time dipping 15 minutes, and executing roll compacting power is 0.9kg/cm2, liquid carrying rate is 70%, puts in baking oven 80 DEG C of preliminary dryings 5 minutes, then
Bake at a temperature of 160 DEG C 3 minutes, after being washed to neutrality, dry at a temperature of 80 DEG C.
Following table is that the modification fabric sample to above-described embodiment is dyed, crease-resistant and the detection data of antibacterial experiment
Table,
。
Dyeability therein test is:
Wherein the dyeing prescription of reactive dye is:
The refined lattice red BF-3B 2%(o.w.f. of element)
Soda Na2CO3 20g/L
Matrii Sulfas Exsiccatus Na2SO4 30g/L
Bath raio 30:1
Dyeing with the dyeing curve shown in Fig. 1, its washing post processing is: add the soap flakes of 3g/l, at 95 DEG C
At a temperature of boil 5 minutes, airing after washing, obtain test sample.
Wrinkle resistance therein is tested:
Select YG (B) 541E type Full automatic digital formula fabric crease elasticity test instrument.Method of testing: the crease resistance folding of fabric
Wrinkle recovery angle represents.This experiment uses and presses the assay method of creasy recovery angle by GB/T 3819-1997, " textile fabric
The mensuration of crease recovery replys horn cupping " in normal beam technique be measured.
Anti-microbial property therein is tested: use " the evaluation of antibacterial textile performance the 3rd of GB GB/T20944.3-2008
Point: concussion method " to test, test strain is gram positive bacteria staphylococcus aureus and gram negative bacteria large intestine bar
Bacterium.Sample bacteriostasis rate computing formula is as follows:
In formula: Y is bacteriostasis rate (%)；Wb is the viable bacteria concentration (CFU/mL) after blank sample oscillating contact 18 h in flask；
Wc is the viable bacteria concentration (CFU/mL) after fabric sample oscillating contact 18 h to be measured in flask.
Claims (8)
1. an amino acid nano-silver modification agent, it is characterised in that the agent of this modification is the most miscible by silver solution and aminoacid
Liquid presses the mixing of 1:1 volume ratio, prepares after stirring 30 ~ 45 minutes at a temperature of 95 ~ 100 DEG C simultaneously, and described silver-colored solution is 0.01 ~
The silver nitrate aqueous solution of 0.05g/L mass concentration scope, the equal miscible fluid of described aminoacid be amino acid solution, cross-linking agent and
The mixed solution that is uniformly dispersed of surfactant, the mass concentration of amino acid solution therein is 20 ~ 60 g/L, and cross-linking agent selects
With one of fatty alcohol glycidyl ether or polybasic carboxylic acid, mass concentration is 20 ~ 60 g/L, and surfactant is fatty alcohol polyoxy
Vinyl Ether, its mass concentration is 2 ~ 6 g/L.
Amino acid nano-silver modification agent the most according to claim 1, it is characterised in that described fatty alcohol shrinks sweet
Oil ether is hexylene glycol glycidyl ether, butanediol diglycidyl ether, propylene glycol diglycidylether, ethylene glycol diglycidyl
In ether one of arbitrarily.
Amino acid nano-silver modification agent the most according to claim 1, it is characterised in that described polybasic carboxylic acid is fourth
In alkane tetrabasic carboxylic acid, citric acid, poly one of arbitrarily.
Amino acid nano-silver modification agent the most according to claim 1, it is characterised in that described surfactant is
In Span-80, Tween80, JFC, paregal O one of arbitrarily.
Amino acid nano-silver modification agent the most according to claim 1, it is characterised in that described amino acid solution
For in lysine solution, glutamic acid aqueous solution or methionine aqueous solution any one.
6. a preparation method for one of arbitrarily described amino acid nano-silver modification agent, its feature in claim 1 to 5
It is that the method is: the equal miscible fluid of aminoacid is mixed by 1:1 volume ratio with silver solution, stirs 30 at a temperature of 95 ~ 100 DEG C simultaneously
~ 45 minutes, prepare, wherein, the described silver nitrate aqueous solution that silver-colored solution is 0.01 ~ 0.05g/L mass concentration scope, described
The equal miscible fluid of aminoacid is the mixed solution that is uniformly dispersed of amino acid solution, cross-linking agent and surfactant, amino therein
The mass concentration of aqueous acid is 20 ~ 60 g/L, and cross-linking agent selects one of fatty alcohol glycidyl ether or polybasic carboxylic acid, quality
Concentration is 20 ~ 60 g/L, and surfactant is fatty alcohol-polyoxyethylene ether, and its mass concentration is 2 ~ 6 g/L.
7. the modification applying in claim 1 to 5 one of arbitrarily described amino acid nano-silver modification agent to obtain is whole
Reason fabric, it is characterised in that this modification fabric is to prepare by the following method: corpus fibrosum or corpus fibrosum fabric immerse amino
In acid nanometer silver modification agent, its bath raio is 1: 30, rolls through two leachings two, every time dipping 15 minutes, and liquid carrying rate is 70 ~ 90%, after
Preliminary drying 5 minutes in 40 ~ 80 DEG C of temperature, then bake 3 minutes through 80 ~ 160 DEG C of temperature, it is washed to neutrality, drying.
Modification fabric the most according to claim 7, it is characterised in that described corpus fibrosum or corpus fibrosum fabric are cotton
Fiber, viscose fiber, tencel fiber, Modal fibre, bamboo fibre, flaxen fiber or its fabric.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105064008A (en) * | 2015-08-22 | 2015-11-18 | 赵兵 | Preparation method and application of nano-silver particles |
| CN105088755A (en) * | 2015-08-22 | 2015-11-25 | 赵兵 | Preparation method and application of silver nano-particles |
| CN105133300A (en) * | 2015-08-22 | 2015-12-09 | 钱景 | Method for preparing nanosilver and finishing fabric |
| CN105133299A (en) * | 2015-08-22 | 2015-12-09 | 赵兵 | Method for preparing nanosilver from honey and finishing cotton linen bamboo fiber fabric |
| CN105088754A (en) * | 2015-08-22 | 2015-11-25 | 赵兵 | Method for preparing nano-silver and nano-silver antibacterial fabric by honey |
| CN105088753A (en) * | 2015-08-22 | 2015-11-25 | 赵兵 | Method for preparing nano-silver and nano-silver antibacterial cotton/linen/bamboo fiber blended fabric by tablet |
| CN105177994B (en) * | 2015-09-25 | 2017-06-06 | 浙江德清恒锦时装有限公司 | A kind of cashmere sweater of air-permeable anti-bacterial |
| CN109403026A (en) * | 2018-10-31 | 2019-03-01 | 嘉兴珠韵服装有限公司 | A kind of preparation method of dyeing and finishing technology pretreating reagent |
| CN112575409A (en) * | 2020-12-01 | 2021-03-30 | 江苏合源纺织科技有限公司 | Flame-retardant cotton-like polyester-nylon composite superfine fiber and production method thereof |
| CN112796105A (en) * | 2020-12-31 | 2021-05-14 | 砾维(新乡)纺织有限公司 | Production process of pure cotton CP flame-retardant fabric |
| CN115160453B (en) * | 2022-07-11 | 2023-04-07 | 东华大学 | Preparation method and application of biomolecule-based chelating film-forming agent |
| CN116556051A (en) * | 2023-05-19 | 2023-08-08 | 珠海厚洺服饰有限公司 | Antioxidation silver fiber fabric |
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| CN103981698A (en) * | 2013-02-07 | 2014-08-13 | 无锡市顺业科技有限公司 | Nano silver antibacterial finishing agent and preparation method thereof |
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| JP2002079269A (en) * | 2000-09-05 | 2002-03-19 | Toray Ind Inc | Silver capturing agent, column for capturing, and silver capturing method |
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| CN1341358A (en) * | 2000-09-07 | 2002-03-27 | 刘建忠 | Silver zinc combined antimicrobial agent |
| CN103981698A (en) * | 2013-02-07 | 2014-08-13 | 无锡市顺业科技有限公司 | Nano silver antibacterial finishing agent and preparation method thereof |
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