CN117587541B - Antibacterial polyamide fiber fabric - Google Patents
Antibacterial polyamide fiber fabric Download PDFInfo
- Publication number
- CN117587541B CN117587541B CN202410067454.4A CN202410067454A CN117587541B CN 117587541 B CN117587541 B CN 117587541B CN 202410067454 A CN202410067454 A CN 202410067454A CN 117587541 B CN117587541 B CN 117587541B
- Authority
- CN
- China
- Prior art keywords
- antibacterial
- polyamide
- modifier
- fiber fabric
- antibacterial polyamide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000004952 Polyamide Substances 0.000 title claims abstract description 106
- 229920002647 polyamide Polymers 0.000 title claims abstract description 106
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 83
- 239000000835 fiber Substances 0.000 title claims abstract description 62
- 239000004744 fabric Substances 0.000 title claims abstract description 40
- 239000003607 modifier Substances 0.000 claims abstract description 39
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 21
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 239000000178 monomer Substances 0.000 claims abstract description 4
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 30
- LCFVJGUPQDGYKZ-UHFFFAOYSA-N Bisphenol A diglycidyl ether Chemical compound C=1C=C(OCC2OC2)C=CC=1C(C)(C)C(C=C1)=CC=C1OCC1CO1 LCFVJGUPQDGYKZ-UHFFFAOYSA-N 0.000 claims description 26
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 22
- IRAGEBXSFXWYNX-UHFFFAOYSA-N 2-(1,3,5-triazinan-1-yl)ethanol Chemical compound OCCN1CNCNC1 IRAGEBXSFXWYNX-UHFFFAOYSA-N 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 17
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 13
- 238000007142 ring opening reaction Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000002074 melt spinning Methods 0.000 claims description 10
- 238000009987 spinning Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 150000001412 amines Chemical class 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 8
- 238000005096 rolling process Methods 0.000 claims description 8
- 230000000845 anti-microbial effect Effects 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000002981 blocking agent Substances 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- 238000004804 winding Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 21
- 230000008569 process Effects 0.000 abstract description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- 238000009941 weaving Methods 0.000 description 7
- 125000003700 epoxy group Chemical group 0.000 description 4
- 238000009940 knitting Methods 0.000 description 4
- 238000009740 moulding (composite fabrication) Methods 0.000 description 4
- 239000003242 anti bacterial agent Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- 239000004599 antimicrobial Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229940113115 polyethylene glycol 200 Drugs 0.000 description 1
- -1 triazine compound Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/48—Polymers modified by chemical after-treatment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
- Polyamides (AREA)
Abstract
The invention relates to an antibacterial polyamide fiber fabric which is woven by antibacterial polyamide fibers, and the preparation method of the antibacterial polyamide fibers comprises the following steps: s1, preparing a modifier HE; s2, preparing a polyamide prepolymer; s3, preparing an antibacterial polyamide material; s4, preparing the antibacterial polyamide fiber. The antibacterial polyamide fiber fabric is woven by antibacterial polyamide fibers, the antibacterial polyamide fibers are prepared by taking laurolactam as a polyamide monomer and sebacic acid as a dicarboxylic acid end-capping agent, the prepared modifier HE is added in the process to serve as an antibacterial modifier, and the prepared fabric is excellent in antibacterial performance and high in strength.
Description
Technical Field
The invention relates to the field of fabrics, in particular to an antibacterial polyamide fiber fabric.
Background
With the continuous development of science and technology, the textile fabric layers meeting different needs of people are endless so as to meet the needs of consumers, and play an increasingly important role in daily life of people. Most of the existing fabrics are woven by adopting single fabric fibers, so that the functions are single, the antibacterial effect is poor, and the use requirements of people cannot be met when the fabric is used.
Antibacterial textiles are usually realized by adding antibacterial agents into textiles, and the preparation method mainly comprises a fibril method and a post-finishing method. The fibril method is to add an antibacterial agent into spinning solution, and the antibacterial fiber is prepared by a spinning process. The finishing method is to attach an antibacterial agent to the surface of the fiber by a coating or padding method to give antibacterial effect to the fabric, and the method is the most studied antibacterial fabric preparation method at present because of simple operation, but the antibacterial durability of the fabric prepared by the method needs to be further improved.
Therefore, there is a need to develop a fiber that does not decrease the fiber strength and also has a better antimicrobial performance for preparing an antimicrobial fabric.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide an antibacterial polyamide fiber fabric.
The aim of the invention is realized by adopting the following technical scheme:
an antibacterial polyamide fiber fabric is woven by adopting antibacterial polyamide fibers, and the preparation method of the antibacterial polyamide fibers comprises the following steps:
s1, preparing a modifier HE:
bisphenol A diglycidyl ether and hydroxyethyl hexahydro s-triazine are weighed to react under the action of an organic amine catalyst, and a modifier HE is prepared;
s2, preparing a polyamide prepolymer:
dodecalactam is used as a polyamide monomer, sebacic acid is used as a blocking agent, and the polyamide prepolymer is obtained through reaction under the action of a ring opening agent;
s3, preparing an antibacterial polyamide material:
mixing and reacting a modifier HE and a polyamide prepolymer to obtain an antibacterial polyamide material;
s4, preparing antibacterial polyamide fibers:
and (3) carrying out melt spinning on the antibacterial polyamide material, stretching, rolling, cooling and forming to form the antibacterial polyamide fiber.
Preferably, the step S1 includes:
weighing bisphenol A diglycidyl ether and an organic amine catalyst, mixing the mixture into Tetrahydrofuran (THF), uniformly stirring the mixture in a reflux device, gradually dropwise adding hydroxyethyl hexahydro s-triazine at 40-60 ℃, continuously stirring the mixture after the dropwise adding is finished for 3-6 hours, and removing impurities through pressure reduction to obtain the modifier HE.
Preferably, the molar ratio of bisphenol A diglycidyl ether and hydroxyethyl hexahydros-triazine of step S1 is 3-3.4:1.
Preferably, the organic amine catalyst in the step S1 is one of triethylamine, dimethylamine and pyridine, and the adding amount of the organic amine catalyst is 3-8% of the mass of the bisphenol A diglycidyl ether.
Preferably, the dripping speed of the step S1 is 40-80 drops/min, and the stirring speed of the reaction liquid is 100-140r/min.
Preferably, the step S2 includes:
mixing sebacic acid and laurolactam into a reaction kettle, adding a ring-opening agent, introducing nitrogen to replace air in the reaction kettle, controlling the pressure in the reaction kettle to be 0.2-0.6MPa and the temperature to be 250-260 ℃, reacting for 2-3 hours, reducing the pressure to normal pressure, vacuumizing, continuing to react for 1-2 hours, reducing the pressure and reducing the temperature to obtain the polyamide prepolymer.
Preferably, the ring-opening agent in the step S2 is deionized water, and the addition amount is 2% -6% of the mass of the laurolactam.
Preferably, the stirring speed of the step S2 is 100-200r/min.
Preferably, the sebacic acid addition amount of the S2 step is 10-15% of the mass of the dodecalactam.
Preferably, the step S3 includes:
mixing modifier HE and polyamide prepolymer into a reaction kettle, heating to 250-260 ℃ under vacuum condition, preserving heat and stirring for 1-1.5h, and reducing pressure and cooling after the reaction is finished to obtain the antibacterial polyamide material.
Preferably, the modifier HE added in the step S3 accounts for 20-50% of the mass of the polyamide prepolymer.
Preferably, the temperature of the melt spinning in the step S4 is 275-290 ℃, the spinning speed is 1400-2000m/min, and the aperture of the spinneret plate is 0.5-0.7mm.
Preferably, the air temperature of the cooling molding in the step S4 is 20-25 ℃, the air speed is 0.5-1m/S, and the relative humidity is 65% -75%.
Preferably, the stretching temperature of the stretching winding in the step S4 is 80-120 ℃ and the stretching multiple is 8-10 times.
Preferably, the antibacterial polyamide fiber is woven into the fabric, and is prepared by weaving the antibacterial polyamide fiber into yarns and then weaving the yarns through one-to-one warps and wefts on a knitting machine.
Preferably, in the weaving process of the fabric, the warp yarn linear density is 32-38tex, and the weft yarn linear density is 20-26tex.
Preferably, in the fabric weaving process, the warp density of the fabric is 98-106 pieces/inch, and the weft density of the fabric is 85-96 pieces/inch.
The beneficial effects of the invention are as follows:
1. the antibacterial polyamide fiber fabric is woven by antibacterial polyamide fibers, the antibacterial polyamide fibers are prepared by taking laurolactam as a polyamide monomer and sebacic acid as a dicarboxylic acid end-capping agent, the prepared modifier HE is added in the process to serve as an antibacterial modifier, and the prepared fabric is excellent in antibacterial performance and high in strength.
2. The invention is characterized in that the modifier HE for preparing the antibacterial polyamide fiber is prepared by combining hydroxyethyl hexahydro s-triazine and bisphenol A diglycidyl ether. Hydroxyethyl hexahydro s-triazine is a triazine compound containing three hydroxyl groups, and bisphenol a diglycidyl ether is a compound containing bis-epoxy groups. In the combining process, after the epoxy group of the bisphenol A diglycidyl ether is ring-opened under alkaline condition, the bisphenol A diglycidyl ether is grafted with the hydroxyl group in the hydroxyethyl hexahydro s-triazine, so that the modifier HE is prepared, and the bisphenol A diglycidyl ether is rich in epoxy groups because unreacted epoxy groups remain.
3. The invention prepares the antibacterial polyamide material by using the prepared modifier HE to replace the traditional glycol and combining with the polyamide prepolymer after ring opening. The principle is that the epoxy group in the modifier HE and the carboxyl group in the polyamide prepolymer are combined and reacted under high temperature and high pressure, so that the triazine group with strong antibacterial property is introduced.
Detailed Description
The technical scheme of the invention is described below through specific examples. It is to be understood that the mention of one or more method steps of the present invention does not exclude the presence of other method steps before and after the combination step or that other method steps may be interposed between these explicitly mentioned steps; it should also be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Moreover, unless otherwise indicated, the numbering of the method steps is merely a convenient tool for identifying the method steps and is not intended to limit the order of arrangement of the method steps or to limit the scope of the invention in which the invention may be practiced, as such changes or modifications in their relative relationships may be regarded as within the scope of the invention without substantial modification to the technical matter.
Wherein, the molecular formula structures of the hydroxyethyl hexahydro-s-triazine, bisphenol A diglycidyl ether and the prepared modifier HE are as follows in sequence:
the molecular formula structure of the hydroxyethyl hexahydro s-triazine is as follows:
；
the molecular formula structure of bisphenol A diglycidyl ether is:
；
the molecular structural formula of the modifier HE is as follows:
。
in order to better understand the above technical solution, exemplary embodiments of the present invention are described in more detail below. While exemplary embodiments of the invention are shown, it should be understood that the invention may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
The invention is further described with reference to the following examples.
Example 1
An antibacterial polyamide fiber fabric is prepared by spinning antibacterial polyamide fibers into yarns, wherein the warp yarn linear density is 35tex, the weft yarn linear density is 22tex, and the yarns are woven on a knitting machine through one-to-one warp and weft weaving; the warp density of the fabric was 102 pieces/inch and the weft density was 88 pieces/inch.
The preparation method of the antibacterial polyamide fiber comprises the following steps:
s1, preparing a modifier HE:
mixing bisphenol A diglycidyl ether and triethylamine into Tetrahydrofuran (THF), wherein the addition amount of the triethylamine is 5 percent of the mass of the bisphenol A diglycidyl ether, the mass ratio of the hydroxyethyl hexahydro-s-triazine to the tetrahydrofuran is 1:6, uniformly stirring in a reflux device, gradually dropwise adding the hydroxyethyl hexahydro-s-triazine under the condition of 45 ℃, wherein the molar ratio of the bisphenol A diglycidyl ether to the hydroxyethyl hexahydro-s-triazine is 3.2:1, the dropwise adding speed is 60 drops/min, continuing stirring for 4 hours after the dropwise adding, the stirring speed is 120r/min, and obtaining the modifier HE after the decompression and impurity removal.
S2, preparing a polyamide prepolymer:
mixing sebacic acid and laurolactam into a reaction kettle, wherein the addition amount of the sebacic acid is 12% of the mass of the laurolactam, adding deionized water as a ring-opening agent, wherein the addition amount is 4% of the mass of the laurolactam, introducing nitrogen to replace air in the reaction kettle, controlling the pressure in the reaction kettle to be 0.4MPa, controlling the temperature to be 250 ℃, and the stirring speed to be 150r/min, reacting for 2 hours, reducing the pressure to normal pressure, vacuumizing, continuing to react for 2 hours, and reducing the pressure and the temperature to obtain the polyamide prepolymer;
s3, preparing an antibacterial polyamide material:
mixing a modifier HE and a polyamide prepolymer into a reaction kettle, wherein the adding amount of the modifier HE is 30% of the mass of the polyamide prepolymer, heating to 250 ℃ under vacuum, preserving heat and stirring for 1h, and reducing the pressure and the temperature after the reaction is finished to obtain an antibacterial polyamide material;
s4, preparing antibacterial polyamide fibers:
carrying out melt spinning on the antibacterial polyamide material, wherein the temperature of the melt spinning is 275-290 ℃, the spinning speed is 1600m/min, the aperture of a spinneret plate is 0.6mm, the stretching and rolling are carried out, the stretching temperature of the stretching and rolling is 100 ℃, the stretching multiple is 9 times, the cooling and forming are carried out, the air temperature is 20-25 ℃, the air speed is 0.6m/s, and the relative humidity is 65% -75%, so that the antibacterial polyamide fiber is formed.
Example 2
An antibacterial polyamide fiber fabric is prepared by spinning antibacterial polyamide fibers into yarns, wherein the warp yarn linear density is 32tex, the weft yarn linear density is 20tex, and the yarns are woven on a knitting machine through one-to-one warp and weft weaving; the warp density of the fabric was 98 pieces/inch and the weft density was 85 pieces/inch.
The preparation method of the antibacterial polyamide fiber comprises the following steps:
s1, preparing a modifier HE:
weighing bisphenol A diglycidyl ether and triethylamine, mixing the bisphenol A diglycidyl ether and the triethylamine into Tetrahydrofuran (THF), wherein the addition amount of the triethylamine is 3 percent of the mass of the bisphenol A diglycidyl ether, uniformly stirring in a reflux device, gradually dropwise adding hydroxyethyl hexahydro s-triazine under the condition of 40 ℃, keeping stirring for 3-6 hours after the dropwise adding is finished, and obtaining a modifier HE after the decompression and impurity removal; the molar ratio of bisphenol A diglycidyl ether to hydroxyethyl hexahydro-s-triazine is 3:1 and the mass ratio of hydroxyethyl hexahydro-s-triazine to tetrahydrofuran is 1:6.
S2, preparing a polyamide prepolymer:
mixing sebacic acid and laurolactam into a reaction kettle, wherein the addition amount of the sebacic acid is 10% of the mass of the laurolactam, adding deionized water as a ring-opening agent, wherein the addition amount is 2% of the mass of the laurolactam, introducing nitrogen to replace air in the reaction kettle, controlling the pressure in the reaction kettle to be 0.2MPa, controlling the temperature to be 250 ℃, and the stirring speed to be 100r/min, reducing the pressure to normal pressure after 2 hours of reaction, vacuumizing to continue the reaction for 1 hour, and reducing the pressure and the temperature to obtain the polyamide prepolymer;
s3, preparing an antibacterial polyamide material:
mixing a modifier HE and a polyamide prepolymer into a reaction kettle, wherein the adding amount of the modifier HE is 20% of the mass of the polyamide prepolymer, heating to 250 ℃ under vacuum, preserving heat and stirring for 1h, and reducing the pressure and the temperature after the reaction is finished to obtain an antibacterial polyamide material;
s4, preparing antibacterial polyamide fibers:
carrying out melt spinning on the antibacterial polyamide material, wherein the temperature of the melt spinning is 275 ℃, the spinning speed is 1400m/min, the aperture of a spinneret plate is 0.5mm, the stretching and rolling are carried out, the stretching temperature of the stretching and rolling is 80 ℃, the stretching multiple is 8 times, the cooling and forming are carried out, the air temperature is 20-25 ℃, the air speed is 0.5m/s, and the relative humidity is 65% -75%, so that the antibacterial polyamide fiber is formed.
Example 3
An antibacterial polyamide fiber fabric is prepared by spinning antibacterial polyamide fibers into yarns, wherein the warp yarn linear density is 38tex, the weft yarn linear density is 26tex, and the yarns are woven on a knitting machine through one-to-one warp and weft weaving; the warp density of the fabric was 106 pieces/inch and the weft density was 96 pieces/inch.
The preparation method of the antibacterial polyamide fiber comprises the following steps:
s1, preparing a modifier HE:
weighing bisphenol A diglycidyl ether and triethylamine, mixing the bisphenol A diglycidyl ether and the triethylamine into Tetrahydrofuran (THF), wherein the addition amount of the triethylamine is 8 percent of the mass of the bisphenol A diglycidyl ether, uniformly stirring in a reflux device, gradually dropwise adding hydroxyethyl hexahydro s-triazine under the condition of 60 ℃, wherein the dropwise adding speed is 80 drops/min, continuing stirring for reaction for 6h after the dropwise adding is finished, and the stirring speed is 140r/min, and obtaining a modifier HE after reducing pressure and removing impurities; the molar ratio of bisphenol A diglycidyl ether to hydroxyethyl hexahydro-s-triazine is 3.4:1 and the mass ratio of hydroxyethyl hexahydro-s-triazine to tetrahydrofuran is 1:6.
S2, preparing a polyamide prepolymer:
mixing sebacic acid and laurolactam into a reaction kettle, wherein the addition amount of the sebacic acid is 15% of the mass of the laurolactam, adding deionized water as a ring-opening agent, wherein the addition amount is 6% of the mass of the laurolactam, introducing nitrogen to replace air in the reaction kettle, controlling the pressure in the reaction kettle to be 0.6MPa, controlling the temperature to be 260 ℃, and the stirring speed to be 200r/min, reacting for 3 hours, reducing the pressure to normal pressure, vacuumizing, continuing to react for 2 hours, and reducing the pressure and the temperature to obtain the polyamide prepolymer;
s3, preparing an antibacterial polyamide material:
mixing a modifier HE and a polyamide prepolymer into a reaction kettle, wherein the adding amount of the modifier HE is 50% of the mass of the polyamide prepolymer, heating to 260 ℃ under vacuum, preserving heat and stirring for 1.5h, and reducing the pressure and the temperature after the reaction is finished to obtain an antibacterial polyamide material;
s4, preparing antibacterial polyamide fibers:
carrying out melt spinning on the antibacterial polyamide material, wherein the temperature of the melt spinning is 275-290 ℃, the spinning speed is 2000m/min, the aperture of a spinneret plate is 0.7mm, the stretching and rolling temperature is 120 ℃, the stretching multiple of the stretching and rolling is 10 times, the cooling and forming are carried out, the air temperature is 20-25 ℃, the air speed is 1m/s, and the relative humidity is 65% -75%, so that the antibacterial polyamide fiber is formed.
Comparative example 1
An antibacterial polyamide fiber was prepared by a method differing from example 1 in that no modifier HE was added.
Comparative example 2
The process for the preparation of the antibacterial polyamide fiber differs from example 1 in that the modifier HE is replaced by hydroxyethyl hexahydros-triazine.
Comparative example 3
An antibacterial polyamide fiber is prepared by a method different from example 1 in that the modifier HE is replaced with polyethylene glycol 200.
The antibacterial polyamide fibers prepared in example 1 and comparative examples 1 to 3 were subjected to performance test, and the results are shown in Table 1.
In Table 1, the detection of breaking strength and breaking elongation is referred to GB/T14337-2022, and the evaluation of bacteriostasis rate of coliform bacteria and staphylococcus aureus is referred to GB/T20944.3-2007.
TABLE 1 Performance detection of different fibers
| Example 1 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Breaking strength (cN/dtex) | 5.6 | 5.8 | 5.0 | 5.2 |
| Elongation at break (%) | 34.6 | 36.1 | 27.2 | 28.9 |
| Coliform bacteria inhibition rate (%) | 92.8 | 67.3 | 90.3 | 69.4 |
| Staphylococcus aureus antibacterial rate (%) | 94.5 | 71.6 | 91.5 | 73.2 |
As can be seen from Table 1, the polyamide fiber prepared in example 1 of the present invention has high breaking strength and elongation at break while maintaining a good antibacterial effect.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms should not be understood as necessarily being directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Further, one skilled in the art can engage and combine the different embodiments or examples described in this specification.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (10)
1. The antibacterial polyamide fiber fabric is characterized by being woven by adopting antibacterial polyamide fibers, and the preparation method of the antibacterial polyamide fibers comprises the following steps of:
s1, preparing a modifier HE:
bisphenol A diglycidyl ether and hydroxyethyl hexahydro s-triazine are weighed to react under the action of an organic amine catalyst, and a modifier HE is prepared;
s2, preparing a polyamide prepolymer:
dodecalactam is used as a polyamide monomer, sebacic acid is used as a blocking agent, and the polyamide prepolymer is obtained through reaction under the action of a ring opening agent;
s3, preparing an antibacterial polyamide material:
mixing and reacting a modifier HE and a polyamide prepolymer to obtain an antibacterial polyamide material;
s4, preparing antibacterial polyamide fibers:
after melt spinning, stretching and rolling the antibacterial polyamide material, and cooling and forming to form antibacterial polyamide fibers;
the molecular structural formula of the modifier HE is as follows:
。
2. the antimicrobial polyamide fiber fabric of claim 1, wherein the step S1 comprises:
weighing bisphenol A diglycidyl ether and an organic amine catalyst, mixing the mixture into Tetrahydrofuran (THF), uniformly stirring the mixture in a reflux device, gradually dropwise adding hydroxyethyl hexahydro s-triazine at 40-60 ℃, continuously stirring the mixture after the dropwise adding is finished for 3-6 hours, and removing impurities through pressure reduction to obtain the modifier HE.
3. The antimicrobial polyamide fiber fabric of claim 2, wherein the mole ratio of bisphenol a diglycidyl ether and hydroxyethyl hexahydros-triazine of step S1 is 3-3.4:1.
4. The antibacterial polyamide fiber fabric according to claim 2, wherein the organic amine catalyst in the step S1 is one of triethylamine, dimethylamine and pyridine, and the addition amount of the organic amine catalyst is 3% -8% of the mass of bisphenol a diglycidyl ether.
5. The antimicrobial polyamide fiber fabric of claim 1, wherein the step S2 comprises:
mixing sebacic acid and laurolactam into a reaction kettle, adding a ring-opening agent, introducing nitrogen to replace air in the reaction kettle, controlling the pressure in the reaction kettle to be 0.2-0.6MPa and the temperature to be 250-260 ℃, reacting for 2-3 hours, reducing the pressure to normal pressure, vacuumizing, continuing to react for 1-2 hours, reducing the pressure and reducing the temperature to obtain the polyamide prepolymer.
6. The antibacterial polyamide fiber fabric according to claim 5, wherein the ring-opening agent in the step S2 is deionized water, and the addition amount of the ring-opening agent is 2-6% of the mass of the laurolactam.
7. The antibacterial polyamide fiber fabric according to claim 5, wherein the amount of sebacic acid added in the step S2 is 10% -15% of the mass of dodecalactam.
8. The antimicrobial polyamide fiber fabric of claim 1, wherein the step S3 comprises:
mixing modifier HE and polyamide prepolymer into a reaction kettle, heating to 250-260 ℃ under vacuum condition, preserving heat and stirring for 1-1.5h, and reducing pressure and cooling after the reaction is finished to obtain the antibacterial polyamide material.
9. The antibacterial polyamide fiber fabric according to claim 8, wherein the modifier HE added in the step S3 is 20-50% of the mass of the polyamide prepolymer.
10. The antibacterial polyamide fiber fabric according to claim 1, wherein the temperature of the melt spinning in the step S4 is 275-290 ℃, the spinning speed is 1400-2000m/min, and the spinneret aperture is 0.5-0.7mm; cooling to 20-25deg.C with wind speed of 0.5-1m/s; the stretching temperature of the stretching winding is 80-120 ℃ and the stretching multiple is 8-10 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410067454.4A CN117587541B (en) | 2024-01-17 | 2024-01-17 | Antibacterial polyamide fiber fabric |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410067454.4A CN117587541B (en) | 2024-01-17 | 2024-01-17 | Antibacterial polyamide fiber fabric |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN117587541A CN117587541A (en) | 2024-02-23 |
| CN117587541B true CN117587541B (en) | 2024-04-05 |
Family
ID=89913644
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410067454.4A Active CN117587541B (en) | 2024-01-17 | 2024-01-17 | Antibacterial polyamide fiber fabric |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117587541B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118064996B (en) * | 2024-04-16 | 2024-06-14 | 比音勒芬服饰股份有限公司 | Portable wear-resistant polyamide fiber fabric |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4606972A (en) * | 1985-09-09 | 1986-08-19 | Allied Corporation | Polyamide yarn with antioxidant finish |
| CN103270086A (en) * | 2010-12-24 | 2013-08-28 | 富士胶片株式会社 | Polyamide polymer, method for producing same, resin composition, molded product, fiber, film, and porous film |
| CN111394868A (en) * | 2020-03-18 | 2020-07-10 | 张海军 | Anti-infection antibacterial fabric for infants and preparation method thereof |
| CN112900085A (en) * | 2021-01-28 | 2021-06-04 | 宁波共振服饰有限公司 | Waterproof and breathable water sports suit fabric and preparation method thereof |
| CN113502660A (en) * | 2021-09-10 | 2021-10-15 | 南通三田纺织有限公司 | Cool antibacterial mosquito net fabric and preparation method thereof |
| CN117107388A (en) * | 2023-09-27 | 2023-11-24 | 东莞信鸿工程塑料有限公司 | Antibacterial flame-retardant polyamide fiber material and preparation method thereof |
| CN117188152A (en) * | 2023-09-13 | 2023-12-08 | 西北工业大学宁波研究院 | Preparation method of antibacterial barrier polyamide fiber |
-
2024
- 2024-01-17 CN CN202410067454.4A patent/CN117587541B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4606972A (en) * | 1985-09-09 | 1986-08-19 | Allied Corporation | Polyamide yarn with antioxidant finish |
| CN103270086A (en) * | 2010-12-24 | 2013-08-28 | 富士胶片株式会社 | Polyamide polymer, method for producing same, resin composition, molded product, fiber, film, and porous film |
| CN111394868A (en) * | 2020-03-18 | 2020-07-10 | 张海军 | Anti-infection antibacterial fabric for infants and preparation method thereof |
| CN112900085A (en) * | 2021-01-28 | 2021-06-04 | 宁波共振服饰有限公司 | Waterproof and breathable water sports suit fabric and preparation method thereof |
| CN113502660A (en) * | 2021-09-10 | 2021-10-15 | 南通三田纺织有限公司 | Cool antibacterial mosquito net fabric and preparation method thereof |
| CN117188152A (en) * | 2023-09-13 | 2023-12-08 | 西北工业大学宁波研究院 | Preparation method of antibacterial barrier polyamide fiber |
| CN117107388A (en) * | 2023-09-27 | 2023-11-24 | 东莞信鸿工程塑料有限公司 | Antibacterial flame-retardant polyamide fiber material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| /TTNO-WPU棉织物抗菌性能研究;刘海生 等;化纤与纺织技术;20231231;第第52 卷卷(第第12期期);第21-25页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN117587541A (en) | 2024-02-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN117587541B (en) | Antibacterial polyamide fiber fabric | |
| CN111918990B (en) | Polyamide fiber, woven and knitted fabric, and method for producing polyamide fiber | |
| US8957179B2 (en) | Shape memory polyamide and method of producing shape memory polyamide fabric using the same | |
| US11053387B2 (en) | One-step spun composite DTY and preparation method thereof | |
| CN102505520A (en) | Functional fabric | |
| CN108138388B (en) | Polyurethane or polyurethane urea elastic yarn having improved colorability and method for preparing the same | |
| CN116926764A (en) | Antibacterial, moisture-absorbing, sweat-releasing and quick-drying knitted material and knitted sweater | |
| CN114451608B (en) | Antibacterial degradable polylactic acid protective clothing | |
| CN111979591B (en) | High-strength high-heat-resistance fine single-fiber nylon 66 fiber and preparation method thereof | |
| TW201821477A (en) | Nylon polymer | |
| CN111607834A (en) | Preparation method of high-performance nylon thermal fuse | |
| CN109610039B (en) | Preparation method of polyurethane urea elastic fiber with high heat setting efficiency | |
| CN111058149B (en) | Biomass polyester and polyamide blended fabric and preparation method and product thereof | |
| KR101964552B1 (en) | Copolymerized polyamide filament having improved hygroscopic property | |
| CN112048780A (en) | Preparation method of wear-resistant washable antibacterial fabric | |
| CN118064996B (en) | Portable wear-resistant polyamide fiber fabric | |
| CN111053312A (en) | Anti-radiation antibacterial fabric | |
| CN118272957B (en) | Carbon dioxide-based polycarbonate fiber and preparation method thereof | |
| CN114293278B (en) | Polyamide 5X fully drawn yarn and preparation method and application thereof | |
| CN118326552B (en) | Composite environment-friendly vamp material and production process thereof | |
| CN111979597B (en) | Method for preparing thermal fuse | |
| CN113882060B (en) | Breathable durable cotton tencel nylon stretch fabric and preparation method thereof | |
| JPH11229272A (en) | Knitted union fabric and its production | |
| CN117926568A (en) | Ultra-low denier nylon composite fabric and production process thereof | |
| KR19980016615A (en) | Spinning apparatus for polymer solution and fabrication method using the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |