CN107881597A - A kind of waterproof fibre for outdoor shoe and preparation method thereof - Google Patents
A kind of waterproof fibre for outdoor shoe and preparation method thereof Download PDFInfo
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- CN107881597A CN107881597A CN201711280897.8A CN201711280897A CN107881597A CN 107881597 A CN107881597 A CN 107881597A CN 201711280897 A CN201711280897 A CN 201711280897A CN 107881597 A CN107881597 A CN 107881597A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0084—Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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Abstract
The invention belongs to fibre technology field, and in particular to a kind of waterproof fibre for outdoor shoe and preparation method thereof.The invention provides a kind of preparation method of the waterproof fibre for outdoor shoe, comprise the following steps：S1 is sodium alginate-modified；It is prepared by S2 polyurethane solutions；S3 PLAs are crosslinked；It is prepared by S4 spinning solutions；S5 wet spinnings, are produced.Waterproof fibre for outdoor shoe prepared by the present invention has preferable waterproof, moisture-inhibiting and antibacterial effect, and adhesional wetting property is 0g, and resistance to net hydraulic pressure value is up to 3650mmH2More than O, penetrability are up to 2840g/m2/ more than 24h, antibiotic rate are up to 99%, and Environmental Safety is comfortable wear-resisting.
Description
Technical field
The invention belongs to fibre technology field, and in particular to a kind of waterproof fibre for outdoor shoe and preparation method thereof.
Background technology
With the progress of living standard, outdoor activities are liked by increasing people, and therefore, the requirement to outdoor shoe is got over
Carry out higher, especially sleety weather, waterproof, moisture-inhibiting must can not.Outdoor shoe includes shoes body, interlayer, waterproof fibre, to long-term
Carry out for outdoor activities and the outdoor fan of amount of exercise greatly, it is impossible to cleaning in time, the growth of bacterium can be caused for a long time, it is right
Human body is unfavorable.The waterproof of outdoor shoe waterproof fibre, water vapour permeability have much room for improvement at present, and anti-microbial property is poor, are unfavorable for growing
Phase outdoor activities, while the washability of existing waterproof fibre is also bad, therefore, develops a kind of waterproof, moisture-inhibiting, antibacterial, and it is washable
The preferable waterproof fibre of property is necessary.
Chinese patent application CN106400150A discloses a kind of waterproof fibre for textile cloth braiding, including following matter
Measure the component of number：50 ~ 80 parts of aluminum oxide, 50 ~ 60 parts of aluminium hydroxide, 40 ~ 60 parts of acetate fiber, 150 ~ 200 parts
Kaolin, 100 ~ 120 parts of cordierite, but the invention waterproof and tensile property have much room for improvement, and moisture-inhibiting and antibacterial ability compared with
Difference.
Chinese patent application CN105291519A discloses a kind of waterproof nano fiber composite fabric, including precoat, its
It is characterised by, the precoat upper surface is provided with waterproof fibre layer, and the waterproof fibre layer is made up of warp thread and weft yarns,
The warp thread is fluoropolymer nanofiber, and the weft yarn is chemical-fibres filaments.But the invention waterproof fibre layer waterproof, thoroughly
Wet, stretching and anti-microbial property have much room for improvement.
The content of the invention
In order to solve problems of the prior art, it is an object of the invention to provide a kind of waterproof for outdoor shoe
Fiber and preparation method thereof.Waterproof fibre for outdoor shoe prepared by the present invention has preferable waterproof, moisture-inhibiting and antibacterial effect
Fruit, Environmental Safety are comfortable wear-resisting.
The invention provides a kind of preparation method of the waterproof fibre for outdoor shoe, comprise the following steps：
S1 adds 1-3g prepared RHIZOMA COPTIDIS with vino in 30-50mL water, is heated to 60-80 DEG C, ultrasonic extraction 1-2h, stirring adds 20-40mL
Thionyl chloride and 5-9g sodium alginates, ultrasonic reaction 0.5-1.5h, rear radiation treatment, obtain modified sodium alginate solution；
10-14g polypropylene glycols are placed in vacuum distillation apparatus by S2, are dehydrated 1-2h in 90kPa, 100-120 DEG C, are cooled to 25-
35 DEG C, 1-3g toluene di-isocyanate(TDI)s and 4-6mL DMFs are added, stirring reaction 1-2h, is heated to 60-
80 DEG C, warm 2-3h is held, 0.5-1.5g Isosorbide-5-Nitraes-fourth dioxane is added, obtains polyurethane solutions；
2-6g PLAs are added in the 40-60mL 1- butyl -3- methylimidazole villaumite aqueous solution by S3, are stirred, then are added
Enter 0.1-0.3g dialkyl peroxides and 1-2g repefrals, be heated to 20-40 DEG C, stirring reaction 30-
50min, obtain cross-linking polylactic acid solution；
S4 will be crosslinked poly- breast obtained by modified sodium alginate solution, step S2 gained polyurethane solutions and step S3 obtained by step S1
Acid solution is well mixed, radiation treatment, and stirring adds 5-10mL aqueous gelatin solutions, obtains spinning solution；
Spinning solution obtained by step S4 is carried out wet spinning by S5, is produced.
Further, radiation treatment is that radiation source is in the step S160Co- gamma-rays, irradiation dose 2-4kGy.
Further, in the step S3 1- butyl -3- methylimidazole villaumites aqueous solution by 1- butyl -3- methylimidazole chlorine
Salt is with water by weight 3-5:10 compositions.
Further, modified sodium alginate solution, polyurethane solutions and cross-linking polylactic acid solution press weight in the step S4
Measure ratio 1:2:1 composition.
Further, radiation treatment is that radiation source is in the step S460Co- gamma-rays, irradiation dose 1-5kGy.
Further, in the step S4 aqueous gelatin solution by gelatin and water by weight 3-4:10 compositions.
Further, wet spinning condition is in the step S5：Spinning temperature is 80-100 DEG C, and coagulating bath is chlorination
Calcium-ethanol-sodium hydroxide solution, coagulation bath temperature are 20-30 DEG C, setting time 3-5min, draw ratio 2-4.
Further, the calcium chloride-ethanol-sodium hydroxide solution by calcium chloride, ethanol and mass concentration be 4% hydrogen
Sodium hydroxide solution is by weight 1:3:2 compositions.
Step S1 of the present invention sodium alginate has been carried out in the presence of dimethyl sulfoxide it is hydrophobic modified, furthermore, prepared RHIZOMA COPTIDIS with vino
Not only colouring and immersion to fiber can also be played to sodium alginate-modified, so as to further improve its antibacterial
Property；Meanwhile the active ingredient jamaicin in prepared RHIZOMA COPTIDIS with vino of the present invention and sodium alginate graft reaction under irradiation, the derivative of formation
But preferable anti-microbial property has unexpectedly been reached.Step S4 of the present invention is molten to modified sodium alginate made from step S1 under irradiation
Cross-linking polylactic acid solution carries out cross-linking reaction made from polyurethane solutions made from liquid, step S2 and S3, and water-soluble by gelatin
Liquid is adjusted the performance of fiber, and waterproof fibre made from wet spinning has preferable mechanical performance, Waterproof Breathable and antibacterial
Effect.Wherein, prepared RHIZOMA COPTIDIS with vino is purchased from the favorable to the people prepared slices of Chinese crude drugs Co., Ltd in Sichuan；Polypropylene glycol CAS：25322-69-4 is purchased from Shanghai wheat
Crin biochemical technology Co., Ltd；PLA CAS：31852-84-3 is purchased from Shanghai Losec Chemical Co., Ltd.；Gelatin CAS：
9000-70-8 is purchased from Shanghai Mike's woods biochemical technology Co., Ltd.
Compared with prior art, the present invention has the advantage that：
（1）Waterproof fibre produced by the present invention for outdoor shoe has good waterproof, water vapour permeability, and adhesional wetting property is 0g, resistance to
Net hydraulic pressure value is up to 3650mmH2More than O, penetrability are up to 2840g/m2/ more than 24h；
（2）Waterproof fibre produced by the present invention for outdoor shoe has excellent antibacterial action, to staphylococcus aureus
Bacteriostasis rate is up to more than 99.3%, is up to more than 99.4% to the bacteriostasis rate of Escherichia coli, the bacteriostasis rate of Candida albicans is up to
More than 98.5%, and there is permanent antibacterial effect still more than 95.2% using bacteriostasis rate after 30 days；
（3）Waterproof fibre produced by the present invention for outdoor shoe passes through modified sodium alginate solution, polyurethane solutions and crosslinking
PLA solution is crosslinked, and spinning is made, and fiber waterproof effect is resistance to caused by overcoming existing composite material and soaking finishing agent
The shortcomings that with property difference；
（4）Waterproof fibre safety and comfort produced by the present invention for outdoor shoe, environmental protection is degradable, wear-resisting.
Embodiment
Below by specific embodiment the present invention will be further explained explanation, these embodiments are only used for the mesh of illustration
, it is not intended to limit protection scope of the present invention.
A kind of preparation method of the waterproof fibre for outdoor shoe of embodiment 1
S1 adds 1g prepared RHIZOMA COPTIDIS with vino in 30mL water, is heated to 60 DEG C, ultrasonic extraction 1h, stirring adds 20mL thionyl chlorides and 5g
Sodium alginate, ultrasonic reaction 0.5h, rear radiation treatment, radiation source are60Co- gamma-rays, irradiation dose 2kGy, obtain modified marine alga
Acid sodium solution；
10g polypropylene glycols are placed in vacuum distillation apparatus by S2, in 90kPa, 100 DEG C of dehydration 1h, are cooled to 25 DEG C, are added
1g toluene di-isocyanate(TDI)s and 4mL DMFs, stirring reaction 1h, are heated to 60 DEG C, hold warm 2h, add
0.5g Isosorbide-5-Nitraes-fourth dioxane, obtain polyurethane solutions；
2g PLAs are added in the 40mL 1- butyl -3- methylimidazole villaumite aqueous solution by S3,1- butyl -3- methylimidazole chlorine
Saline solution is by 1- butyl -3- methylimidazole villaumites and water by weight 3:10 compositions, stir, add 0.1g dialkyl group
Peroxide and 1g repefrals, 20 DEG C are heated to, stirring reaction 30min, obtains cross-linking polylactic acid solution；
S4 will be crosslinked poly- breast obtained by modified sodium alginate solution, step S2 gained polyurethane solutions and step S3 obtained by step S1
Acid solution is by weight 1:2:1 is well mixed, radiation treatment, and radiation source is60Co- gamma-rays, irradiation dose 1kGy, stirring add
Enter 5mL aqueous gelatin solutions, aqueous gelatin solution is by gelatin and water by weight 3:10 compositions, obtain spinning solution；
Spinning solution obtained by step S4 is carried out wet spinning by S5, and spinning temperature is 80 DEG C, and coagulating bath is calcium chloride-ethanol-hydrogen
Sodium hydroxide solution, wherein calcium chloride-ethanol-sodium hydroxide solution by calcium chloride, ethanol and mass concentration be 4% sodium hydroxide
Solution is by weight 1:3:2 compositions, coagulation bath temperature are 20 DEG C, setting time 3min, draw ratio 2, are produced.
A kind of preparation method of the waterproof fibre for outdoor shoe of embodiment 2
S1 adds 2g prepared RHIZOMA COPTIDIS with vino in 40mL water, is heated to 70 DEG C, ultrasonic extraction 1.5h, stirring add 30mL thionyl chlorides and
7g sodium alginates, ultrasonic reaction 1h, rear radiation treatment, radiation source are60Co- gamma-rays, irradiation dose 3kGy, obtain modified marine alga
Acid sodium solution；
12g polypropylene glycols are placed in vacuum distillation apparatus by S2, in 90kPa, 110 DEG C of dehydration 1.5h, are cooled to 30 DEG C, then add
Enter 2g toluene di-isocyanate(TDI)s and 5mL DMFs, stirring reaction 1.5h, be heated to 70 DEG C, hold warm 2.5h, then
1.0g Isosorbide-5-Nitraes-fourth dioxane is added, obtains polyurethane solutions；
4g PLAs are added in the 50mL 1- butyl -3- methylimidazole villaumite aqueous solution by S3,1- butyl -3- methylimidazole chlorine
Saline solution is by 1- butyl -3- methylimidazole villaumites and water by weight 4:10 compositions, stir, add 0.2g dialkyl group
Peroxide and 1.5g repefrals, 30 DEG C are heated to, stirring reaction 40min, obtains cross-linking polylactic acid solution；
S4 will be crosslinked poly- breast obtained by modified sodium alginate solution, step S2 gained polyurethane solutions and step S3 obtained by step S1
Acid solution is by weight 1:2:1 is well mixed, radiation treatment, and radiation source is60Co- gamma-rays, irradiation dose 3kGy, stirring add
Enter 7.5mL aqueous gelatin solutions, aqueous gelatin solution is by gelatin and water by weight 3.5:10 compositions, obtain spinning solution；
Spinning solution obtained by step S4 is carried out wet spinning by S5, and spinning temperature is 90 DEG C, and coagulating bath is calcium chloride-ethanol-hydrogen
Sodium hydroxide solution, wherein calcium chloride-ethanol-sodium hydroxide solution by calcium chloride, ethanol and mass concentration be 4% sodium hydroxide
Solution is by weight 1:3:2 compositions, coagulation bath temperature are 25 DEG C, setting time 4min, draw ratio 3, are produced.
A kind of preparation method of the waterproof fibre for outdoor shoe of embodiment 3
S1 adds 3g prepared RHIZOMA COPTIDIS with vino in 50mL water, is heated to 80 DEG C, ultrasonic extraction 2h, stirring adds 40mL thionyl chlorides and 9g
Sodium alginate, ultrasonic reaction 1.5h, rear radiation treatment, radiation source are60Co- gamma-rays, irradiation dose 4kGy, obtain modified marine alga
Acid sodium solution；
14g polypropylene glycols are placed in vacuum distillation apparatus by S2, in 90kPa, 120 DEG C of dehydration 2h, are cooled to 35 DEG C, are added
3g toluene di-isocyanate(TDI)s and 6mL DMFs, stirring reaction 2h, are heated to 80 DEG C, hold warm 3h, add
1.5g Isosorbide-5-Nitraes-fourth dioxane, obtain polyurethane solutions；
6g PLAs are added in the 60mL 1- butyl -3- methylimidazole villaumite aqueous solution by S3,1- butyl -3- methylimidazole chlorine
Saline solution is by 1- butyl -3- methylimidazole villaumites and water by weight 5:10 compositions, stir, add 0.3g dialkyl group
Peroxide and 2g repefrals, 40 DEG C are heated to, stirring reaction 50min, obtains cross-linking polylactic acid solution；
S4 will be crosslinked poly- breast obtained by modified sodium alginate solution, step S2 gained polyurethane solutions and step S3 obtained by step S1
Acid solution is by weight 1:2:1 is well mixed, radiation treatment, and radiation source is60Co- gamma-rays, irradiation dose 5kGy, stirring add
Enter 10mL aqueous gelatin solutions, aqueous gelatin solution is by gelatin and water by weight 4:10 compositions, obtain spinning solution；
Spinning solution obtained by step S4 is carried out wet spinning by S5, and spinning temperature is 100 DEG C, coagulating bath be calcium chloride-ethanol-
Sodium hydroxide solution, wherein calcium chloride-ethanol-sodium hydroxide solution by calcium chloride, ethanol and mass concentration be 4% hydroxide
Sodium solution is by weight 1:3:2 compositions, coagulation bath temperature are 30 DEG C, setting time 5min, draw ratio 4, are produced.
A kind of preparation method of the waterproof fibre for outdoor shoe of comparative example 1
S1 adds 7g sodium alginates in 40mL water, is heated to 70 DEG C, stirs, obtains modified sodium alginate solution；
12g polypropylene glycols are placed in vacuum distillation apparatus by S2, in 90kPa, 110 DEG C of dehydration 1.5h, are cooled to 30 DEG C, then add
Enter 2g toluene di-isocyanate(TDI)s and 5mL DMFs, stirring reaction 1.5h, be heated to 70 DEG C, hold warm 2.5h, then
1.0g Isosorbide-5-Nitraes-fourth dioxane is added, obtains polyurethane solutions；
4g PLAs are added in the 50mL 1- butyl -3- methylimidazole villaumite aqueous solution by S3,1- butyl -3- methylimidazole chlorine
Saline solution is by 1- butyl -3- methylimidazole villaumites and water by weight 4:10 compositions, stir, add 0.2g dialkyl group
Peroxide and 1.5g repefrals, 30 DEG C are heated to, stirring reaction 40min, obtains cross-linking polylactic acid solution；
S4 will be crosslinked poly- breast obtained by modified sodium alginate solution, step S2 gained polyurethane solutions and step S3 obtained by step S1
Acid solution is by weight 1:2:1 is well mixed, radiation treatment, and radiation source is60Co- gamma-rays, irradiation dose 3kGy, stirring add
Enter 7.5mL aqueous gelatin solutions, aqueous gelatin solution is by gelatin and water by weight 3.5:10 compositions, obtain spinning solution；
Spinning solution obtained by step S4 is carried out wet spinning by S5, and spinning temperature is 90 DEG C, and coagulating bath is calcium chloride-ethanol-hydrogen
Sodium hydroxide solution, wherein calcium chloride-ethanol-sodium hydroxide solution by calcium chloride, ethanol and mass concentration be 4% sodium hydroxide
Solution is by weight 1:3:2 compositions, coagulation bath temperature are 25 DEG C, setting time 4min, draw ratio 3, are produced.
Difference with embodiment 2 is, sodium alginate is not modified.
A kind of preparation method of the waterproof fibre for outdoor shoe of comparative example 2
S1 adds the 2g coptiss in 40mL water, is heated to 70 DEG C, ultrasonic extraction 1.5h, stirring adds 30mL thionyl chlorides and 7g
Sodium alginate, ultrasonic reaction 1h, rear radiation treatment, radiation source are60Co- gamma-rays, irradiation dose 3kGy, obtain modified alginic acid
Sodium solution；
12g polypropylene glycols are placed in vacuum distillation apparatus by S2, in 90kPa, 110 DEG C of dehydration 1.5h, are cooled to 30 DEG C, then add
Enter 2g toluene di-isocyanate(TDI)s and 5mL DMFs, stirring reaction 1.5h, be heated to 70 DEG C, hold warm 2.5h, then
1.0g Isosorbide-5-Nitraes-fourth dioxane is added, obtains polyurethane solutions；
4g PLAs are added in the 50mL 1- butyl -3- methylimidazole villaumite aqueous solution by S3,1- butyl -3- methylimidazole chlorine
Saline solution is by 1- butyl -3- methylimidazole villaumites and water by weight 4:10 compositions, stir, add 0.2g dialkyl group
Peroxide and 1.5g repefrals, 30 DEG C are heated to, stirring reaction 40min, obtains cross-linking polylactic acid solution；
S4 will be crosslinked poly- breast obtained by modified sodium alginate solution, step S2 gained polyurethane solutions and step S3 obtained by step S1
Acid solution is by weight 1:2:1 is well mixed, radiation treatment, and radiation source is60Co- gamma-rays, irradiation dose 3kGy, stirring add
Enter 7.5mL aqueous gelatin solutions, aqueous gelatin solution is by gelatin and water by weight 3.5:10 compositions, obtain spinning solution；
Spinning solution obtained by step S4 is carried out wet spinning by S5, and spinning temperature is 90 DEG C, and coagulating bath is calcium chloride-ethanol-hydrogen
Sodium hydroxide solution, wherein calcium chloride-ethanol-sodium hydroxide solution by calcium chloride, ethanol and mass concentration be 4% sodium hydroxide
Solution is by weight 1:3:2 compositions, coagulation bath temperature are 25 DEG C, setting time 4min, draw ratio 3, are produced.
Difference with embodiment 2 is, the prepared RHIZOMA COPTIDIS with vino in step S1 is replaced with into the coptis.
A kind of preparation method of the waterproof fibre for outdoor shoe of comparative example 3
S1 adds 2g prepared RHIZOMA COPTIDIS with vino in 40mL water, is heated to 70 DEG C, ultrasonic extraction 1.5h, stirring add 30mL thionyl chlorides and
7g sodium alginates, ultrasonic reaction 1h, rear radiation treatment, radiation source are60Co- gamma-rays, irradiation dose 3kGy, obtain modified marine alga
Acid sodium solution；
12g polypropylene glycols are placed in vacuum distillation apparatus by S2, in 90kPa, 110 DEG C of dehydration 1.5h, are cooled to 30 DEG C, then add
Enter 2g toluene di-isocyanate(TDI)s and 5mL DMFs, stirring reaction 1.5h, be heated to 70 DEG C, hold warm 2.5h, then
1.0g Isosorbide-5-Nitraes-fourth dioxane is added, obtains polyurethane solutions；
4g PLAs are added in the 50mL 1- butyl -3- methylimidazole villaumite aqueous solution by S3,1- butyl -3- methylimidazole chlorine
Saline solution is by 1- butyl -3- methylimidazole villaumites and water by weight 4:10 compositions, stir, add 0.2g dialkyl group
Peroxide and 1.5g repefrals, 30 DEG C are heated to, stirring reaction 40min, obtains cross-linking polylactic acid solution；
S4 will be crosslinked poly- breast obtained by modified sodium alginate solution, step S2 gained polyurethane solutions and step S3 obtained by step S1
Acid solution is by weight 1:2:1 is well mixed, and stirring adds 7.5mL aqueous gelatin solutions, and aqueous gelatin solution is by gelatin and water by weight
Measure ratio 3.5:10 compositions, obtain spinning solution；
Spinning solution obtained by step S4 is carried out wet spinning by S5, and spinning temperature is 90 DEG C, and coagulating bath is calcium chloride-ethanol-hydrogen
Sodium hydroxide solution, wherein calcium chloride-ethanol-sodium hydroxide solution by calcium chloride, ethanol and mass concentration be 4% sodium hydroxide
Solution is by weight 1:3:2 compositions, coagulation bath temperature are 25 DEG C, setting time 4min, draw ratio 3, are produced.
Difference with embodiment 2 is that modified sodium alginate solution, polyurethane solutions and cross-linking polylactic acid are molten in step S4
Liquid does not do radiation treatment.
Test example one, tensile property test
According to GB/T19975-2005《High-strength chemical-fibre filament draw method for testing performance》To embodiment 1-3 and comparative example 1-3 systems
The tensile property test of the standby waterproof fibre for outdoor shoe, the results are shown in Table 1.
The tensile property test result of table 1
| Group | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Line density/dtex | 1.11 | 1.03 | 1.18 | 1.60 | 1.42 | 1.76 |
| Fracture strength/CNdtex-1 | 2.91 | 3.12 | 2.86 | 2.43 | 2.58 | 2.31 |
| Elongation at break/% | 19.6 | 20.4 | 19.1 | 15.7 | 16.9 | 15.1 |
As shown in Table 1, the tensile property of the waterproof fibre for outdoor shoe prepared by the present invention is preferable.Compared with comparative example 1-3,
To sodium alginate-modified in waterproof fibre for outdoor shoe prepared by the embodiment of the present invention 2, and each component spoke in step S4
It is more preferable according to the tensile property of fiber made from processing.
Test example two, waterproofing and moisture-penetration performances test
According to GB/T4744-1997《Textile fabric water permeability resistance determines》、GB/T12704《Textile fabric penetrability experiment side
Method》The waterproofing and moisture-penetration performances of the waterproof fibre for outdoor shoe prepared by embodiment 1-3 and comparative example 1-3 are determined, are as a result seen
Table 2.
The waterproofing and moisture-penetration performances test result of table 2
As shown in Table 2, the waterproof fibre waterproofing and moisture-penetration performances for outdoor shoe that prepared by the present invention are preferable.With comparative example 1-3 groups
Contrast, the waterproof fibre waterproofing and moisture-penetration performances for outdoor shoe prepared by 1-3 of embodiment of the present invention groups are preferable, illustrate present invention system
Each component radiation treatment in the modification of sodium alginate and step S4, can improve fibre in the standby waterproof fibre for outdoor shoe
The waterproof of dimension, water vapour permeability.
Test example three, anti-microbial property test
According to ATCC standards, antibiotic property is carried out to the waterproof fibre for outdoor shoe prepared by embodiment 1-3 and comparative example 1-3
It can test, test result is shown in Table 3.
The anti-microbial property test result of table 3
As shown in Table 3, the waterproof fibre for outdoor shoe that prepared by the present invention has excellent antibacterial action, to golden yellow grape
The bacteriostasis rate of coccus is up to more than 99.3%, more than 99.4% is up to the bacteriostasis rate of Escherichia coli, to the antibacterial of Candida albicans
Rate is up to more than 98.5%.Compared with comparative example 1-3, the waterproof fibre excellent antibacterial effect for outdoor shoe of the invention prepared
Preferably, illustrate that the present invention prepares the active ingredient jamaicin and alginic acid used in the waterproof fibre for outdoor shoe in prepared RHIZOMA COPTIDIS with vino
Sodium reacts under irradiation, and the derivative of generation has got unexpected antibacterial effect.
In addition, after using 30 days the waterproof fibre for outdoor shoe prepared by embodiment 1-3 groups, respectively to golden yellow Portugal
Grape coccus, Escherichia coli and Candida albicans carry out antibacterial tests, the results showed that, with the increase of usage time, anti-microbial property
Can slowly it decline, but using after 30 days, bacteriostasis rate is still more than 95.2%.
To sum up, by test example one, two, three, the embodiment of the present invention 2 is most preferred embodiment, obtained to be used for open air
The waterproof fibre of footwear has optimal mechanical performance, Waterproof Breathable row and antibiotic property.
Claims (9)
1. the preparation method of a kind of waterproof fibre for outdoor shoe, it is characterised in that comprise the following steps：
S1 adds 1-3g prepared RHIZOMA COPTIDIS with vino in 30-50mL water, is heated to 60-80 DEG C, ultrasonic extraction 1-2h, stirring adds 20-40mL
Thionyl chloride and 5-9g sodium alginates, ultrasonic reaction 0.5-1.5h, rear radiation treatment, obtain modified sodium alginate solution；
10-14g polypropylene glycols are placed in vacuum distillation apparatus by S2, are dehydrated 1-2h in 90kPa, 100-120 DEG C, are cooled to 25-
35 DEG C, 1-3g toluene di-isocyanate(TDI)s and 4-6mL DMFs are added, stirring reaction 1-2h, is heated to 60-
80 DEG C, warm 2-3h is held, 0.5-1.5g Isosorbide-5-Nitraes-fourth dioxane is added, obtains polyurethane solutions；
2-6g PLAs are added in the 40-60mL 1- butyl -3- methylimidazole villaumite aqueous solution by S3, are stirred, then are added
Enter 0.1-0.3g dialkyl peroxides and 1-2g repefrals, be heated to 20-40 DEG C, stirring reaction 30-
50min, obtain cross-linking polylactic acid solution；
S4 will be crosslinked poly- breast obtained by modified sodium alginate solution, step S2 gained polyurethane solutions and step S3 obtained by step S1
Acid solution is well mixed, radiation treatment, and stirring adds 5-10mL aqueous gelatin solutions, obtains spinning solution；
Spinning solution obtained by step S4 is carried out wet spinning by S5, is produced.
2. it is used for the preparation method of the waterproof fibre of outdoor shoe as claimed in claim 1, it is characterised in that in the step S1
Radiation treatment is that radiation source is60Co- gamma-rays, irradiation dose 2-4kGy.
3. it is used for the preparation method of the waterproof fibre of outdoor shoe as claimed in claim 1, it is characterised in that in the step S3
1- butyl -3- methylimidazole villaumites the aqueous solution is by 1- butyl -3- methylimidazole villaumites and water by weight 3-5:10 compositions.
4. it is used for the preparation method of the waterproof fibre of outdoor shoe as claimed in claim 1, it is characterised in that in the step S4
Modified sodium alginate solution, polyurethane solutions and cross-linking polylactic acid solution are by weight 1:2:1 composition.
5. it is used for the preparation method of the waterproof fibre of outdoor shoe as claimed in claim 1, it is characterised in that in the step S4
Radiation treatment is that radiation source is60Co- gamma-rays, irradiation dose 1-5kGy.
6. it is used for the preparation method of the waterproof fibre of outdoor shoe as claimed in claim 1, it is characterised in that in the step S4
Aqueous gelatin solution is by gelatin and water by weight 3-4:10 compositions.
7. it is used for the preparation method of the waterproof fibre of outdoor shoe as claimed in claim 1, it is characterised in that in the step S5
Wet spinning condition is：Spinning temperature is 80-100 DEG C, and coagulating bath is calcium chloride-ethanol-sodium hydroxide solution, coagulation bath temperature
For 20-30 DEG C, setting time 3-5min, draw ratio 2-4.
8. it is used for the preparation method of the waterproof fibre of outdoor shoe as claimed in claim 7, it is characterised in that the calcium chloride-
Ethanol-sodium hydroxide solution is by sodium hydroxide solution that calcium chloride, ethanol and mass concentration are 4% by weight 1:3:2 compositions.
A kind of 9. obtained waterproof fiber of the preparation method of waterproof fibre for outdoor shoe as described in claim 1-8 is any
Dimension.
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| CN110552083A (en) * | 2018-05-31 | 2019-12-10 | 句容市华冠服帽厂 | Preparation method of antibacterial filament |
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