CN103614927B - A kind of fiber textile containing cellulose antibiotic finishing method - Google Patents
A kind of fiber textile containing cellulose antibiotic finishing method Download PDFInfo
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Abstract
The present invention relates to a kind of fiber textile containing cellulose antibiotic finishing method, the method is with natural high polymer shitosan, sodium alginate for wall material, and Chinese medical extract is core, adopts microcapsules technology, and Chinese medical extract is encapsulated; Then Final finishing mode is adopted by microcapsules process on part carboxy methylation fiber textile containing cellulose, by the electrostatic attraction on cellulose fibre between carboxyl and shitosan, and the crosslinked action of crosslinking agent, the washability that endowing antibacterial can be good.The raw materials used environmental protection of the present invention, safe and efficient, gained textiles has good antibacterial effect to common staphylococcus aureus, Escherichia coli, hay bacillus.
Description
Technical field
The invention belongs to textile technology field, relate to a kind of fiber textile containing cellulose antibiotic finishing method.
Background technology
Textiles is the easy microorganism such as breed bacteria, mould in use; antibacterial fabric not only can effectively prevent textiles to be subject to the infringement of these harmful bacterial classifications; and well can protect the health of user, produce peculiar smell as underwear can be prevented, prevent the growth and breeding of fungi on socks, prevent infant from producing erythema etc. because of touching diaper.
Antiseptic for textiles mainly contains: organic antibacterial agent, inorganic antiseptic, natural antibacterial agent three class.These antiseptics respectively have feature, but are difficult to meet the primary conditions such as wide spectrum, efficient, safe, washable, environmental protection simultaneously.Utilize microcapsules technology to make antibacterial microcapsule by coated for one or more antiseptics, then adopt suitable crosslinking agent to arrange on textiles, can effectively overcome above-mentioned defect, obtain good finishing effect.
Shitosan is unique alkaline polysaccharide that nature exists, and is a kind of nontoxic, good biocompatibility, biodegradable natural macromolecular material.Amino on chitosan molecule chain is positively charged when low pH, these amino can be electronegative with fungal cell surface group effect, thus change mobility and the permeability of pathogen cell membrane, interference DNA copying and transcribing, block the metabolism of pathogen, there is good antibacterial activity.Sodium alginate is the class straight-chain polysaccharide extracted from brown alga, seaweed plant, containing a large amount of carboxyl on its strand.Under certain condition, the amino on chitosan molecule chain can attract to form polyelectrolyte film by positive and negative charge with the carboxyl in sodium alginate strand, and spontaneous formation capsule, this capsule is used widely in medicament slow release preparation.But, the preparation that alginate/chitosan bio-microcapsule is used for antibacterial fabric is had no report up to now.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of fiber textile containing cellulose antibiotic finishing method.The method for wall material, adopts microcapsules technology that Antibacterial Constituents is encapsulated with shitosan, sodium alginate, products obtained therefrom environmental protection, safe and efficient and have broad spectrum antibacterial; By Final finishing mode by antibacterial microcapsule process on textiles, capsule is combined firmly with textiles, and has good washability.
The technical scheme realizing above-mentioned purpose is: to have the natural extract of antibacterial activity for core, natural high polymer shitosan, sodium alginate are wall material, adopts two-step method to prepare alginate/chitosan biological antibiotic microcapsules; Then adopt dipping, the mode process that bakes on part carboxy methylation fiber textile containing cellulose, gained antibacterial fabric has good broad spectrum antibacterial, and washing fastness is excellent.
A kind of fiber textile containing cellulose antibiotic finishing method provided by the invention comprises the following steps:
(1) preparation of alginate/chitosan antibacterial microcapsule: Chinese medical extract being joined 50-100mL mass fraction is in the sodium alginate soln of 2%-4%, fully stirs and evenly mixs.In distance liquid level 10cm eminence, with No. 5 syringe needles by sodium alginate and Chinese medical extract mixed solution, under magnetic stirring, dropwise at the uniform velocity instill the CaCl of mass fraction 1%-3%
2in solution, after continuing to stir 0.5-1.5h, gel micro-ball is leached, with distilled water washing 3-5 time, for subsequent use.Shitosan is dissolved in volume fraction 0.5%-2% acetum, be made into mass fraction 1.5%-3% chitosan solution, then gel micro-ball is joined in chitosan-acetic acid solution, after magnetic agitation 0.5-2h, suction filtration, collects capsule, with distilled water washing 3-5 time, after capsule surface water being blotted with filter paper, be placed in 4 DEG C of refrigerators and preserve stand-by.
(2) preparation of carboxy methylation fiber textile containing cellulose: by 5g textile impregnation in the soda bath of mass fraction 10%-30%, after flooding 15-45min at 20-35 DEG C, fabric is taken out, put into the 100mL finite concentration monoxone aqueous solution, take out after 30-45min, fabric is sealed in polyethylene plastic bag, be placed in 30-80 DEG C of baking oven and react 1-3h, then use ethanol/water mixed solution (V/V=80/20) to wash 3-5 time, dry.
(3) preparation of antibacterial fabric: alginate/chitosan antibacterial microcapsule is dispersed in distilled water, preparation mass concentration 5.0-10.0g/L microcapsules dressing liquid; Above-mentioned carboxy methylation fiber textile containing cellulose is immersed in microcapsules dressing liquid, after dipping 30-45min, takes out, then the cross-linking agent solution of impregnating effect mark 1%-5%, takes out after 0.5-1.5h, after flint dry 5-15min, wash 3-5 time, dry.
As shown from the above technical solution: first the present invention to utilize on chitosan molecule chain carboxyl in primary amine groups and sodium alginate strand to form polyelectrolyte film by positive and negative charge attraction, the characteristic of spontaneous formation capsule, will have the Chinese medical extract microencapsulation of antibacterial activity; Then by fiber textile containing cellulose part carboxy methylation, cellulose fibre strand introduces appropriate carboxyl, utilize the electrostatic attraction on carboxyl and microcapsule wall material-chitosan molecule chain between amino on cellulose fibre strand, by the process of alginate/chitosan antibacterial microcapsule on fiber textile containing cellulose, being cross-linked further by crosslinking agent, improve the binding strength of microcapsules and textiles, reach washable object.
As preferably, the Chinese medical extract described in step (1) is one or more in Honegsukle flower P.E, aloe extract, Folium Artemisiae Argyi extract, phellodendron extract, Baical Skullcap root P.E, nutgall extractive, dandelion extract.
As preferably, the sodium alginate described in step (1) and Chinese medical extract mass ratio are 1:1-4:1.
As preferably, the chitosan molecule amount described in step (1) is 0.5-3.5 × 10
5, deacetylation is 60%-75%.Deacetylating degree of chitosan is too high, and microcapsules adhesion can be made serious, can not be shaping.Deacetylating degree of chitosan is too low, and meeting gained microcapsule wall is too thin.
As preferably, the fiber textile containing cellulose described in step (2) is cotton, fiber crops, viscose fabric, or both intertextures, or the intertexture of they and other fibers.
As preferably, the chloroacetic concentration described in step (2) is relative to the heavy 15%-30% of fabric.Monoxone concentration is too low, carboxymethyl content on cellulose fibre can be made less, affect the binding strength of alginate/chitosan antibacterial microcapsule and textiles; But it is serious that too high monoxone concentration can cause fabric strength to damage.
As preferably, the crosslinking agent described in step (3) is isophorone diisocyanate, 1, the one in hexamethylene-diisocyanate.
As preferably, the flint dry temperature described in step (3) is 80-100 DEG C.
A kind of fiber textile containing cellulose antibiotic finishing method advantage of the present invention is:
(1) using Chinese medical extract as antimicrobial component, natural high polymer shitosan, sodium alginate as the wall material of microcapsules, environmental protection.
(2) adopt microcapsules technology that Chinese medical extract is encapsulated, improve the stability of Chinese medical extract, extend the action time of active ingredient, reduce the excitant of Chinese medical extract.
(3) by the electrostatic attraction on carboxyl, hydroxyl and the shitosan on carboxy methylation containing cellulose fiber fabric between amino, by the crosslinked action of crosslinking agent, improve the binding strength of microcapsules and textiles, give the persistence of antibacterial effect.
Detailed description of the invention
The term used in the present invention, unless otherwise specified, generally has the implication that those of ordinary skill in the art understand usually.
Below in conjunction with specific embodiment, in further detail the present invention is described.Should be understood that these embodiments just in order to demonstrate the invention, but not limit the scope of the invention by any way.
Embodiment 1
(1) 1g Honegsukle flower P.E being joined 50mL mass fraction is in the sodium alginate soln of 2%, fully stirs and evenly mixs.In distance liquid level 10cm eminence, with No. 5 syringe needles by sodium alginate and Honegsukle flower P.E mixed solution, under magnetic stirring, dropwise at the uniform velocity instill the CaCl of mass fraction 1%
2in solution, after continuing to stir 0.5h, gel micro-ball is leached, washs 3 times with distilled water, for subsequent use.By shitosan (molecular weight 0.5 × 10
5deacetylation is 75%) be dissolved in volume fraction 0.5% acetum, be made into mass fraction 1.5% chitosan solution, then gel micro-ball is joined in chitosan-acetic acid solution, after magnetic agitation 0.5h, suction filtration, collect capsule, wash 3 times with distilled water, after capsule surface water being blotted with filter paper, be placed in 4 DEG C of refrigerators and preserve stand-by.
(2) 5g pure cotton fabric is immersed in the soda bath of mass fraction 10%, after flooding 15min at 35 DEG C, fabric is taken out, put into 100mL and weigh the 15% monoxone aqueous solution relative to fabric, take out after 30min, fabric is sealed in polyethylene plastic bag, be placed in 30 DEG C of baking ovens and react 3h, then use ethanol/water mixed solution (V/V=80/20) to wash 3 times, dry.
(3) alginate/chitosan antibacterial microcapsule is dispersed in distilled water, preparation mass concentration 5.0g/L microcapsules dressing liquid; By above-mentioned carboxymethylated cotton textile impregnation in microcapsules dressing liquid, after dipping 30min, take out, then the isophorone diisocyanate solution of impregnating effect mark 1%, takes out after 0.5h, after 80 DEG C of drying 15min, washes 3 times, dries.
Comparative example 1
Adopt the method identical with embodiment 1 to prepare alginate/chitosan antibacterial microcapsule and carboxy methylation COTTON FABRIC, then alginate/chitosan antibacterial microcapsule is dispersed in distilled water, preparation mass concentration 5.0g/L microcapsules dressing liquid; COTTON FABRIC is immersed in microcapsules dressing liquid, after dipping 30min, takes out, after 80 DEG C of drying 15min, wash 3 times, dry.
Embodiment 2
(1) 1g aloe extract being joined 100mL mass fraction is in the sodium alginate soln of 4%, fully stirs and evenly mixs.In distance liquid level 10cm eminence, with No. 5 syringe needles by sodium alginate and Chinese medical extract mixed solution, under magnetic stirring, dropwise at the uniform velocity instill the CaCl of mass fraction 3%
2in solution, after continuing to stir 1.5h, gel micro-ball is leached, washs 5 times with distilled water, for subsequent use.By shitosan (molecular weight 3.5 × 10
5deacetylation is 70%) be dissolved in volume fraction 2% acetum, be made into mass fraction 3% chitosan solution, then gel micro-ball is joined in chitosan-acetic acid solution, after magnetic agitation 2h, suction filtration, collect capsule, wash 5 times with distilled water, after capsule surface water being blotted with filter paper, be placed in 4 DEG C of refrigerators and preserve stand-by.
(2) 5g ramie fabric is immersed in the soda bath of mass fraction 30%, after flooding 45min at 20 DEG C, fabric is taken out, put into 100mL and weigh the 30% monoxone aqueous solution relative to fabric, take out after 45min, fabric is sealed in polyethylene plastic bag, be placed in 80 DEG C of baking ovens and react 1h, then use ethanol/water mixed solution (V/V=80/20) to wash 5 times, dry.
(3) alginate/chitosan antibacterial microcapsule is dispersed in distilled water, preparation mass concentration 10.0g/L microcapsules dressing liquid; Above-mentioned carboxy methylation ramie fabric is immersed in microcapsules dressing liquid, dipping 45min after, take out, then impregnating effect mark 5% 1, hexamethylene-diisocyanate solution, takes out after 1.5h, after 100 DEG C of drying 5min, washes 5 times, dries.
Comparative example 2
Adopt the method identical with embodiment 2 to prepare alginate/chitosan antibacterial microcapsule and carboxy methylation ramie fabric, then alginate/chitosan antibacterial microcapsule is dispersed in distilled water, preparation mass concentration 10.0g/L microcapsules dressing liquid; Ramie fabric is immersed in microcapsules dressing liquid, after dipping 45min, after taking out 100 DEG C of drying 5min, washes 5 times, dry
Embodiment 3
(1) 1g Folium Artemisiae Argyi extract being joined 80mL mass fraction is in the sodium alginate soln of 2.5%, fully stirs and evenly mixs.In distance liquid level 10cm eminence, with No. 5 syringe needles by sodium alginate and Folium Artemisiae Argyi extract mixed solution, under magnetic stirring, dropwise at the uniform velocity instill the CaCl of mass fraction 2%
2in solution, after continuing to stir 1h, gel micro-ball is leached, washs 4 times with distilled water, for subsequent use.By shitosan (molecular weight 1.5 × 10
5deacetylation is 65%) be dissolved in volume fraction 1% acetum, be made into mass fraction 2.5% chitosan solution, then gel micro-ball is joined in chitosan-acetic acid solution, after magnetic agitation 1h, suction filtration, collect capsule, wash 4 times with distilled water, after capsule surface water being blotted with filter paper, be placed in 4 DEG C of refrigerators and preserve stand-by.
(2) 5g viscose fabric is immersed in the soda bath of mass fraction 20%, after flooding 30min at 30 DEG C, fabric is taken out, put into 100mL and weigh the 20% monoxone aqueous solution relative to fabric, take out after 40min, fabric is sealed in polyethylene plastic bag, be placed in 60 DEG C of baking ovens and react 2h, then use ethanol/water mixed solution (V/V=80/20) to wash 4 times, dry.
(3) alginate/chitosan antibacterial microcapsule is dispersed in distilled water, preparation mass concentration 8.0g/L microcapsules dressing liquid; Be immersed in microcapsules dressing liquid by above-mentioned carboxy methylation viscose fabric, after dipping 40min, take out, then the isophorone diisocyanate solution of impregnating effect mark 3%, takes out after 1h, after 90 DEG C of drying 10min, washes 4 times, dries.
Comparative example 3
Adopt the method identical with embodiment 3 to prepare alginate/chitosan antibacterial microcapsule and carboxy methylation viscose fabric, then alginate/chitosan antibacterial microcapsule is dispersed in distilled water, preparation mass concentration 8.0g/L microcapsules dressing liquid; Viscose fabric is immersed in microcapsules dressing liquid, after dipping 40min, takes out, after 90 DEG C of drying 10min, wash 4 times, dry
Embodiment 4
(1) 0.6g phellodendron extract being joined 60mL mass fraction is in the sodium alginate soln of 3%, fully stirs and evenly mixs.In distance liquid level 10cm eminence, with No. 5 syringe needles by sodium alginate and phellodendron extract mixed solution, under magnetic stirring, dropwise at the uniform velocity instill in the CaCl2 solution of mass fraction 1.5%, after continuing to stir 1h, gel micro-ball is leached, 3 times are washed with distilled water, for subsequent use.By shitosan (molecular weight 2.0 × 10
5deacetylation is 68%) be dissolved in volume fraction 1.5% acetum, be made into mass fraction 2% chitosan solution, then gel micro-ball is joined in chitosan-acetic acid solution, after magnetic agitation 1.5h, suction filtration, collect capsule, wash 3 times with distilled water, after capsule surface water being blotted with filter paper, be placed in 4 DEG C of refrigerators and preserve stand-by.
(2) 5g polyester/cotton blended fabric is immersed in the soda bath of mass fraction 25%, after flooding 40min at 25 DEG C, fabric is taken out, put into 100mL and weigh the 25% monoxone aqueous solution relative to fabric, take out after 35min, fabric is sealed in polyethylene plastic bag, be placed in 40 DEG C of baking ovens and react 2.5h, then use ethanol/water mixed solution (V/V=80/20) to wash 3 times, dry.
(3) alginate/chitosan antibacterial microcapsule is dispersed in distilled water, preparation mass concentration 6.0g/L microcapsules dressing liquid; Above-mentioned carboxy methylation polyester/cotton blended fabric is immersed in microcapsules dressing liquid, dipping 30min after, take out, then impregnating effect mark 2% 1, hexamethylene-diisocyanate solution, takes out after 0.5h, after 85 DEG C of drying 15min, washes 3 times, dries.
Comparative example 4
Adopt the method identical with embodiment 4 to prepare alginate/chitosan antibacterial microcapsule and carboxy methylation polyester/cotton blended fabric, then alginate/chitosan antibacterial microcapsule is dispersed in distilled water, preparation mass concentration 6.0g/L microcapsules dressing liquid; Polyester/cotton blended fabric is immersed in microcapsules dressing liquid, after dipping 30min, takes out, after 85 DEG C of drying 15min, wash 3 times, dry.
Embodiment 5
Anti-microbial property is tested: the anti-microbial property measuring finish fabric with reference to FZ/T01021-1992 " antibacterial fabric method for testing performance ", is calculated as follows bacteriostasis rate:
In formula: A-is without the bacterium colony average on antibiotic finish fabric; The bacterium colony average of B-on antibiotic finish fabric.
Antibacterial effect water-wash resistance is tested: the test of fabric anti-bacterial effect water-wash resistance completes in color fastness to washing testing machine, washing procedure following (this washing procedure is equivalent to 5 washings): room temperature, detergent concentration 0.2%, 150mL solution, steel ball 10, washes 45min.Take out sample after washing, clean 2 times in 100mL water, each 1min.
Antibacterial fabric test result is as follows:
The performance test of table 1 antibacterial fabric
As can be seen from the above table, gained alginate/chitosan antibacterial microcapsule has good anti-microbial property, to staphylococcus aureus, Escherichia coli, hay bacillus, there is good antibacterial effect through its finish fabric, and microcapsules are combined with textiles firmly, antibacterial effect has good wash durability.Because fabric in comparative example does not add crosslinking agent without carboxy methylation process, the amount processing the microcapsules on fabric is less, and the combination of microcapsules and fabric is more weak, therefore, compared with embodiment, no matter be that antibiotic property or washing fastness are all poor.
Claims (8)
1. a fiber textile containing cellulose antibiotic finishing method, comprises the following steps:
(1) preparation of alginate/chitosan antibacterial microcapsule: Chinese medical extract being joined 50-100mL mass fraction is in the sodium alginate soln of 2%-4%, fully stirs and evenly mixs; In distance liquid level 10cm eminence, with No. 5 syringe needles by sodium alginate and Chinese medical extract mixed solution, under magnetic stirring, dropwise at the uniform velocity instill the CaCl of mass fraction 1%-3%
2in solution, after continuing to stir 0.5-1.5h, gel micro-ball is leached, with distilled water washing 3-5 time, for subsequent use; Shitosan is dissolved in volume fraction 0.5%-2% acetum, be made into mass fraction 1.5%-3% chitosan solution, then gel micro-ball is joined in chitosan-acetic acid solution, after magnetic agitation 0.5-2h, suction filtration, collects capsule, with distilled water washing 3-5 time, after capsule surface water being blotted with filter paper, be placed in 4 DEG C of refrigerators and preserve stand-by;
(2) preparation of carboxy methylation fiber textile containing cellulose: by 5g textile impregnation in the soda bath of mass fraction 10%-30%, after flooding 15-45min at 20-35 DEG C, fabric is taken out, put into the 100mL finite concentration monoxone aqueous solution, take out after 30-45min, fabric is sealed in polyethylene plastic bag, be placed in 30-80 DEG C of baking oven and react 1-3h, then be that the ethanol of 80:20 and the mixed solution of water wash 3-5 time by volume ratio, dry;
(3) preparation of antibacterial fabric: alginate/chitosan antibacterial microcapsule is dispersed in distilled water, preparation mass concentration 5.0-10.0g/L microcapsules dressing liquid; Above-mentioned carboxy methylation fiber textile containing cellulose is immersed in microcapsules dressing liquid, after dipping 30-45min, takes out, then the cross-linking agent solution of impregnating effect mark 1%-5%, takes out after 0.5-1.5h, after flint dry 5-15min, wash 3-5 time, dry.
2. a kind of fiber textile containing cellulose antibiotic finishing method described in claim 1, is characterized in that: Chinese medical extract is one or more in Honegsukle flower P.E, aloe extract, Folium Artemisiae Argyi extract, phellodendron extract, Baical Skullcap root P.E, nutgall extractive, dandelion extract.
3. a kind of fiber textile containing cellulose antibiotic finishing method described in claim 1, is characterized in that: sodium alginate and Chinese medical extract mass ratio are 1:1-4:1.
4. a kind of fiber textile containing cellulose antibiotic finishing method described in claim 1, is characterized in that: chitosan molecule amount is 0.5-3.5 × 10
5, deacetylation is 60%-75%.
5. a kind of fiber textile containing cellulose antibiotic finishing method described in claim 1, is characterized in that: fiber textile containing cellulose is cotton, fiber crops, viscose fabric, or both intertextures, or the intertexture of they and other fibers.
6. a kind of fiber textile containing cellulose antibiotic finishing method described in claim 1, is characterized in that: chloroacetic concentration is for weighing 15%-30% relative to fabric.
7. a kind of fiber textile containing cellulose antibiotic finishing method described in claim 1, is characterized in that: crosslinking agent is isophorone diisocyanate, 1, the one in hexamethylene-diisocyanate.
8. a kind of fiber textile containing cellulose antibiotic finishing method described in claim 1, is characterized in that: flint dry temperature is 80-100 DEG C.
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