CN118547388B - Antibacterial acrylic fiber - Google Patents
Antibacterial acrylic fiber Download PDFInfo
- Publication number
- CN118547388B CN118547388B CN202410946119.1A CN202410946119A CN118547388B CN 118547388 B CN118547388 B CN 118547388B CN 202410946119 A CN202410946119 A CN 202410946119A CN 118547388 B CN118547388 B CN 118547388B
- Authority
- CN
- China
- Prior art keywords
- polyacrylonitrile
- methacrylic acid
- polyamide
- carbamate
- spinning
- 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
Classifications
-
- 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
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to the technical field of acrylic fibers and discloses an antibacterial acrylic fiber, wherein a polyacrylonitrile copolymer modifier contains a polyacrylonitrile block molecular chain and a carbamate structural unit, so that the polyacrylonitrile copolymer modifier plays a role of a compatilizer, the interfacial compatibility between polyacrylonitrile and polyamide 6 is improved, the polyacrylonitrile and the polyamide 6 are subjected to wet spinning very well, the strength of the polyamide 6 is high, the breaking performance is good, and the breaking strength and the breaking elongation of the acrylic fiber can be effectively improved after the polyacrylonitrile copolymer modifier is blended with the polyacrylonitrile for spinning. The polyacrylonitrile copolymer modifier contains quaternary ammonium salt antibacterial groups, and has good compatibility with polyacrylonitrile, and can be uniformly dispersed in an acrylic fiber matrix after spinning, so that the antibacterial performance of the fiber is remarkably improved.
Description
The application relates to a high-strength antibacterial acrylic fiber and a preparation process, which are respectively applied for the application number 2024106343899, the application date 2024, the 5 th month and the 22 th day and the application name.
Technical Field
The invention relates to the technical field of acrylic fibers, in particular to an antibacterial acrylic fiber.
Background
The acrylic fiber is prepared from polyacrylonitrile serving as a raw material through wet spinning, melt spinning and other processes, and has good heat retention, elasticity, heat resistance and other properties; has wide application in the aspects of clothing, clothes and medical articles. However, the acrylic fiber has lower breaking strength and does not have good antibacterial property, which is not beneficial to the practical application of the acrylic fiber in the fields of medical treatment, health and the like. The polyamide nylon fiber has good wear resistance, high strength and good fracture performance; the polyamide, polyacrylonitrile, cotton fiber, polylactic acid and the like are subjected to blending spinning or blending, so that the fiber material with excellent performance can be obtained. However, the compatibility of polyamide and polyacrylonitrile is poor, and the phase separation phenomenon of blended yarn is obvious, so that the performance of acrylic fiber can be affected. The invention utilizes the polyacrylonitrile copolymer modifier and the polyamide 6 to improve the strength and the antibacterial property of the polyacrylonitrile fiber.
Disclosure of Invention
The invention solves the technical problems that: solves the problem of poor strength and antibacterial property of acrylic fiber.
The technical scheme is as follows: the high-strength antibacterial acrylic fiber is characterized by comprising 100 parts by weight of polyacrylonitrile, 2-10 parts by weight of polyamide 6 and 1-6 parts by weight of polyacrylonitrile copolymer modifier.
Wherein, the preparation process of the high-strength antibacterial acrylic fiber comprises the following steps: adding 100 parts by weight of polyacrylonitrile and 1-6 parts by weight of polyacrylonitrile copolymer modifier into dimethyl sulfoxide, and uniformly stirring to obtain a polyacrylonitrile solution; adding polyamide 6 into dimethyl sulfoxide, and stirring uniformly to obtain a polyamide 6 solution; then adding the polyamide 6 solution into the polyacrylonitrile solution, uniformly mixing, carrying out vacuum deaeration to obtain spinning precursor solution, spinning by adopting a wet spinning machine, wherein the extrusion speed of a spinning injector in the wet spinning machine is 0.4-0.6mL/min; the extruded spinning solution enters a coagulating bath which is a dimethyl sulfoxide aqueous solution with the volume fraction of 50-60% to form nascent fibers, and then the nascent fibers are drafted in a draft box at the temperature of 100-110 ℃, and the high-strength antibacterial acrylic fibers are obtained through heat setting, winding and collecting.
Wherein, the preparation process of the polyacrylonitrile copolymer modifier comprises the following steps:
Adding acrylonitrile and methacrylic acid-2-carbamate quaternary ammonium salt monomer into dimethyl sulfoxide solvent, adding azodiisobutyronitrile in nitrogen atmosphere, carrying out copolymerization reaction for 3-6h at 70-85 ℃, adding ethanol into the solution for precipitation after the reaction, filtering, and washing with ethanol to obtain the polyacrylonitrile copolymer modifier.
Wherein the mass of the methacrylic acid-2-carbamate quaternary ammonium salt and the azodiisobutyronitrile acrylonitrile are respectively 15-40% and 0.9-1.2% of the mass of the acrylonitrile.
Wherein, the preparation process of the methacrylic acid-2-carbamate quaternary ammonium salt monomer comprises the following steps:
And (1) adding methacrylic acid-2-isocyanic acid ethyl ester and 3-dimethylamino-1-propanol into the 1, 4-dioxane solvent, reacting for 3-5h at 60-80 ℃ in nitrogen atmosphere, rotary evaporating, and washing the product with petroleum ether to obtain methacrylic acid-2-carbamate propyl tertiary amine.
And (2) adding methacrylic acid-2-carbamate propyl tertiary amine and bromoalkyl compound into isopropanol, carrying out reflux reaction at 80-85 ℃ for 60-72h, carrying out rotary evaporation, and recrystallizing the product in ethanol to obtain methacrylic acid-2-carbamate quaternary ammonium salt monomer.
Wherein the mass of the 3-dimethylamino-1-propanol in the step (1) is 68-82% of the mass of the ethyl methacrylate-2-isocyanate.
Wherein the mass of the bromoalkyl compound is 160-200% of that of the methacrylic acid-2-carbamate propyl tertiary amine; the bromoalkyl compound is any one of 1-bromododecane, 1-bromotridecane, 1-bromotetradecane, 1-bromopentadecane and 1-bromohexadecane.
The technical effects are as follows: the invention uses methacrylic acid-2-isocyanic acid ethyl ester, 3-dimethylamino-1-propanol and bromoalkyl compound to react, thus obtaining novel methacrylic acid-2-carbamate quaternary ammonium salt monomer, and then the novel methacrylic acid-2-carbamate quaternary ammonium salt monomer is copolymerized with acrylonitrile, thus obtaining the polyacrylonitrile copolymer modifier.
The invention utilizes polyacrylonitrile, polyamide 6 and a polyacrylonitrile copolymer modifier to carry out blending wet spinning, wherein the polyacrylonitrile copolymer modifier contains a polyacrylonitrile block molecular chain, has good similar compatibility with polyacrylonitrile, contains a carbamate structural unit, can form hydrogen bond interaction with an amide bond of the polyamide 6 and has good interface interaction with the polyamide 6, so that the polyacrylonitrile copolymer modifier plays a role of a compatilizer, improves the interface compatibility between the polyacrylonitrile and the polyamide 6, and enables the polyacrylonitrile copolymer modifier and the polyamide 6 to carry out wet spinning very well, thereby avoiding influencing the performance of acrylic fiber due to incompatibility of a spinning system. The polyamide 6 has high strength and good breaking performance, and can effectively improve the breaking strength and breaking elongation of the acrylic fiber after being blended with polyacrylonitrile for spinning.
The polyacrylonitrile copolymer modifier contains quaternary ammonium salt antibacterial groups, and has good compatibility with polyacrylonitrile, and can be uniformly dispersed in an acrylic fiber matrix after spinning, so that the antibacterial performance of the fiber is remarkably improved.
Drawings
FIG. 1 is a reaction scheme for the preparation of a quaternary ammonium methacrylate-2-urethane monomer.
Detailed Description
For further understanding of the present invention, the technical aspects of the present invention will be clearly and fully described in connection with the following embodiments, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The CAS number of the methacrylic acid-2-isocyanatoethyl ester of the embodiment of the invention is 30674-80-7. 3-dimethylamino-1-propanol CAS number 3179-63-3. The CAS number of 1-bromododecane is 143-15-7. The CAS number of 1-bromotetradecane is 112-71-0. The 1-bromohexadecane CAS number is 112-82-3. Polyacrylonitrile, molecular weight 85000, model D12000066.
Example 1
(1) To 15mL of 1, 4-dioxane solvent were added 1g of ethyl methacrylate-2-isocyanatoate and 0.82g of 3-dimethylamino-1-propanol, and the reaction was carried out in a nitrogen atmosphere at 80℃for 3 hours, and rotary evaporation was carried out, and the product was washed with petroleum ether to obtain 2-carbamic acid propyl tertiary amine.
(2) To 12mL of isopropanol were added 1g of 2-carbamic acid ester propyl tertiary amine and 1.6g of 1-bromododecane, and the mixture was refluxed at 85℃for 72 hours, and the product was rotary evaporated and recrystallized in ethanol to obtain 2-carbamic acid ester quaternary ammonium salt monomer of methacrylic acid.
(3) 2G of acrylonitrile and 0.3g of methacrylic acid-2-carbamate quaternary ammonium salt monomer are added into 5mL of dimethyl sulfoxide solvent, 18mg of azodiisobutyronitrile is added into nitrogen atmosphere, copolymerization reaction is carried out for 5h at the temperature of 80 ℃, ethanol is added into the solution for precipitation after the reaction, and the polyacrylonitrile copolymer modifier is obtained after filtration and ethanol washing.
(4) 10G of polyacrylonitrile and 0.1g of polyacrylonitrile copolymer modifier are added into 80mL of dimethyl sulfoxide, and uniformly stirred to obtain a polyacrylonitrile solution; 0.2g of polyamide 6 is added into 5mL of dimethyl sulfoxide and stirred uniformly to obtain a polyamide 6 solution; then adding the polyamide 6 solution into the polyacrylonitrile solution, uniformly mixing, and carrying out vacuum deaeration to obtain spinning precursor solution, spinning by adopting a wet spinning machine, wherein the extrusion speed of a spinning injector in the wet spinning machine is 0.6mL/min; the extruded spinning solution enters a coagulating bath which is a dimethyl sulfoxide aqueous solution with the volume fraction of 55 percent to form nascent fibers, then the nascent fibers are drafted in a draft box at the temperature of 110 ℃ and the draft multiple of 4 times, and the high-strength antibacterial acrylic fibers are obtained through heat setting, winding and collecting.
Example 2
(1) To 10mL of a1, 4-dioxane solvent were added 1g of ethyl methacrylate-2-isocyanatoate and 0.75g of 3-dimethylamino-1-propanol, and the reaction was carried out in a nitrogen atmosphere at 60℃for 5 hours, followed by rotary evaporation, and the product was washed with petroleum ether to obtain 2-carbamic acid propyl tertiary amine.
(2) To 12mL of isopropanol, 1g of methacrylic acid-2-carbamate propyl tertiary amine and 1.78g of 1-bromotetradecane were added, and the mixture was refluxed at 80℃for 72 hours, and the product was rotary evaporated and recrystallized in ethanol to obtain methacrylic acid-2-carbamate quaternary ammonium salt monomer.
(3) 2G of acrylonitrile and 0.5g of methacrylic acid-2-carbamate quaternary ammonium salt monomer are added into 10mL of dimethyl sulfoxide solvent, 20mg of azodiisobutyronitrile is added into nitrogen atmosphere, copolymerization reaction is carried out for 3h at the temperature of 85 ℃, ethanol is added into the solution for precipitation after the reaction, and the polyacrylonitrile copolymer modifier is obtained after filtration and ethanol washing.
(4) 10G of polyacrylonitrile and 0.3g of polyacrylonitrile copolymer modifier are added into 90mL of dimethyl sulfoxide, and uniformly stirred to obtain a polyacrylonitrile solution; 0.6g of polyamide 6 is added into 8mL of dimethyl sulfoxide and stirred uniformly to obtain a polyamide 6 solution; then adding the polyamide 6 solution into the polyacrylonitrile solution, uniformly mixing, and carrying out vacuum deaeration to obtain spinning precursor solution, spinning by adopting a wet spinning machine, wherein the extrusion speed of a spinning injector in the wet spinning machine is 0.6mL/min; the extruded spinning solution enters a coagulating bath which is a dimethyl sulfoxide aqueous solution with the volume fraction of 50 percent to form nascent fibers, then the nascent fibers are drafted in a draft box at the temperature of 110 ℃ and the draft multiple of 4 times, and the high-strength antibacterial acrylic fibers are obtained through heat setting, winding and collecting.
Example 3
(1) To 10mL of a1, 4-dioxane solvent were added 1g of 2-isocyanatoethyl methacrylate and 0.68g of 3-dimethylamino-1-propanol, and the reaction was carried out in a nitrogen atmosphere at 80℃for 4 hours, followed by rotary evaporation, and the product was washed with petroleum ether to obtain 2-carbamic acid propyl tertiary amine.
(2) 1G of methacrylic acid-2-carbamate propyl tertiary amine and 2g of 1-bromohexadecane are added into 15mL of isopropanol, reflux reaction is carried out for 60h at the temperature of 85 ℃, rotary evaporation is carried out, and the product is recrystallized in ethanol to obtain methacrylic acid-2-carbamate quaternary ammonium salt monomer.
(3) 2G of acrylonitrile and 0.8g of methacrylic acid-2-carbamate quaternary ammonium salt monomer are added into 10mL of dimethyl sulfoxide solvent, 24mg of azodiisobutyronitrile is added into nitrogen atmosphere, copolymerization reaction is carried out for 6h at 70 ℃, ethanol is added into the solution for precipitation after the reaction, and the polyacrylonitrile copolymer modifier is obtained after filtration and ethanol washing.
(4) 10G of polyacrylonitrile and 0.6g of polyacrylonitrile copolymer modifier are added into 90mL of dimethyl sulfoxide, and uniformly stirred to obtain a polyacrylonitrile solution; 1g of polyamide 6 is added into 10mL of dimethyl sulfoxide and stirred uniformly to obtain a polyamide 6 solution; then adding the polyamide 6 solution into the polyacrylonitrile solution, uniformly mixing, and carrying out vacuum deaeration to obtain spinning precursor solution, spinning by adopting a wet spinning machine, wherein the extrusion speed of a spinning injector in the wet spinning machine is 0.4mL/min; the extruded spinning solution enters a coagulating bath which is a dimethyl sulfoxide aqueous solution with the volume fraction of 60 percent to form nascent fibers, then the nascent fibers are drafted in a draft box at the temperature of 100 ℃ and the draft multiple of 4 times, and the high-strength antibacterial acrylic fibers are obtained through heat setting, winding and collecting.
The main difference between comparative example 1 and example 1 is that the polyamide 6 solution and the polyacrylonitrile copolymer modifier were not added during spinning.
Adding 10g of polyacrylonitrile into 90mL of dimethyl sulfoxide, stirring uniformly, performing vacuum deaeration to obtain spinning precursor solution, spinning by adopting a wet spinning machine, wherein the extrusion speed of a spinning injector in the wet spinning machine is 0.6mL/min; the extruded spinning solution enters a coagulating bath which is a dimethyl sulfoxide aqueous solution with the volume fraction of 50 percent to form nascent fibers, then the nascent fibers are drafted in a draft box at the temperature of 110 ℃ and the draft multiple of 4 times, and the acrylic fibers are obtained through heat setting, winding and collecting.
The main difference between comparative example 2 and example 1 is that no polyamide 6 solution was added during spinning.
Adding 10g of polyacrylonitrile and 0.3g of polyacrylonitrile copolymer modifier into 90mL of dimethyl sulfoxide, uniformly stirring, and carrying out vacuum defoamation to obtain spinning solution, spinning by adopting a wet spinning machine, wherein the extrusion speed of a spinning injector in the wet spinning machine is 0.6mL/min; the extruded spinning solution enters a coagulating bath which is a dimethyl sulfoxide aqueous solution with the volume fraction of 50 percent to form nascent fibers, then the nascent fibers are drafted in a draft box at the temperature of 110 ℃ and the draft multiple of 4 times, and the acrylic fibers are obtained through heat setting, winding and collecting.
The main difference between comparative example 3 and example 1 is that no polyacrylonitrile copolymer modifier was added during spinning.
10G of polyacrylonitrile is added into 90mL of dimethyl sulfoxide and stirred uniformly to obtain a polyacrylonitrile solution; 0.6g of polyamide 6 is added into 8mL of dimethyl sulfoxide and stirred uniformly to obtain a polyamide 6 solution; then adding the polyamide 6 solution into the polyacrylonitrile solution, uniformly mixing, and carrying out vacuum deaeration to obtain spinning precursor solution, spinning by adopting a wet spinning machine, wherein the extrusion speed of a spinning injector in the wet spinning machine is 0.6mL/min; the extruded spinning solution enters a coagulating bath which is a dimethyl sulfoxide aqueous solution with the volume fraction of 50 percent to form nascent fibers, then the nascent fibers are drafted in a draft box at the temperature of 110 ℃ and the draft multiple of 4 times, and the acrylic fibers are obtained through heat setting, winding and collecting.
The main difference between comparative example 4 and example 1 is that no acrylonitrile was added when preparing the copolymer modifier.
0.3G of methacrylic acid-2-carbamate quaternary ammonium salt monomer is added into 2mL of dimethyl sulfoxide solvent, 18mg of azodiisobutyronitrile is added into nitrogen atmosphere, copolymerization reaction is carried out for 5h at the temperature of 80 ℃, ethanol is added into the solution for precipitation after the reaction, and the copolymer modifier is obtained after filtering and ethanol washing.
10G of polyacrylonitrile and 0.1g of copolymer modifier are added into 80mL of dimethyl sulfoxide, and uniformly stirred to obtain a polyacrylonitrile solution; 0.2g of polyamide 6 is added into 5mL of dimethyl sulfoxide and stirred uniformly to obtain a polyamide 6 solution; then adding the polyamide 6 solution into the polyacrylonitrile solution, uniformly mixing, and carrying out vacuum deaeration to obtain spinning precursor solution, spinning by adopting a wet spinning machine, wherein the extrusion speed of a spinning injector in the wet spinning machine is 0.6mL/min; the extruded spinning solution enters a coagulating bath which is a dimethyl sulfoxide aqueous solution with the volume percentage of 55 percent to form nascent fibers, then the nascent fibers are drafted in a draft box at the temperature of 110 ℃ and the draft multiple of 4 times, and the acrylic fibers are obtained through heat setting, winding and collecting.
The breaking performance of the acrylic fiber is tested by adopting the electronic single fiber strength, the clamping distance is 20mm, and the stretching speed is 20 mm/min. The linear density of the acrylic fiber was 3.33dext.
Taking escherichia coli as a test strain, and performing antibacterial performance test; adding the acrylic fiber after ultraviolet irradiation sterilization into 10 6 CFU/mL of escherichia coli bacterial suspension; shaking at room temperature for 0.5-12h, transferring 0.2mL of bacterial suspension into PBS buffer solution, transferring 0.1mL of bacterial solution, coating on the surface of an agar culture medium, placing into a constant temperature and humidity incubator, culturing at 37 ℃ for 24h, counting viable bacteria after culturing, and calculating the antibacterial rate. Antibacterial ratio= (B-C)/bx 100%, C is the number of bacteria after the culture of the experimental group, B is the number of bacteria of the blank group, and acrylic fiber of comparative example 1 is used as the blank group.
According to the embodiment 1-3, the polyacrylonitrile, the polyamide 6 and the polyacrylonitrile copolymer modifier are used for carrying out blending wet spinning, the polyacrylonitrile copolymer modifier contains a polyacrylonitrile block molecular chain, has good compatibility with polyacrylonitrile, contains a carbamate structural unit, can form hydrogen bond interaction with an amide bond of the polyamide 6, and has good interface interaction with the polyamide 6, so that the polyacrylonitrile copolymer modifier plays a role of a compatilizer, the interface compatibility between the polyacrylonitrile and the polyamide 6 is improved, and the polyacrylonitrile copolymer modifier and the polyamide 6 are subjected to wet spinning very well, and the influence on the performance of acrylic fibers due to incompatibility of a spinning system is avoided. The polyamide 6 has high strength and good breaking performance, and can effectively improve the breaking strength and breaking elongation of the acrylic fiber after being blended with polyacrylonitrile for spinning.
The polyacrylonitrile copolymer modifier contains quaternary ammonium salt antibacterial groups, and has good compatibility with polyacrylonitrile, and can be uniformly dispersed in an acrylic fiber matrix after spinning, so that the antibacterial performance of the fiber is remarkably improved.
Comparative example 1 is a pure polyacrylonitrile fiber, and the breaking strength and the breaking elongation are poor.
Comparative example 2 does not add polyamide 6, the breaking performance of acrylic fiber is poor, but the polyacrylonitrile copolymer modifier is added, and the acrylic fiber has good antibacterial performance because the polyacrylonitrile copolymer modifier contains quaternary ammonium salt antibacterial groups.
Comparative example 3 was free of added polyacrylonitrile copolymer modifier. The compatibility between polyacrylonitrile and polyamide 6 is poor, and interfacial phase separation is easy to generate between the polyacrylonitrile and polyamide 6 in the spinning process, so that the fracture performance of the acrylic fiber can be influenced. And does not contain quaternary ammonium salt antibacterial groups and does not show antibacterial performance.
Comparative example 4 when preparing the copolymer modifier, acrylonitrile was not added. The copolymer modifier does not contain a polyacrylonitrile block molecular chain, has poor compatibility with polyacrylonitrile, does not play a role in compatibilizing the polyacrylonitrile and the polyamide 6, has poor compatibility with the polyamide 6, and can influence the breaking performance of the acrylic fiber, but the copolymer modifier contains a large number of quaternary ammonium salt antibacterial groups, so that the antibacterial performance of the acrylic fiber can be improved.
It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
Claims (2)
1. The antibacterial acrylic fiber is characterized by comprising 100 parts by weight of polyacrylonitrile, 2-10 parts by weight of polyamide 6 and 1-6 parts by weight of polyacrylonitrile copolymer modifier;
The preparation process of the polyacrylonitrile copolymer modifier comprises the following steps: adding acrylonitrile and methacrylic acid-2-carbamate quaternary ammonium salt monomer into dimethyl sulfoxide solvent, adding azodiisobutyronitrile in nitrogen atmosphere, and carrying out copolymerization reaction to obtain polyacrylonitrile copolymer modifier;
The preparation process of the methacrylic acid-2-carbamate quaternary ammonium salt monomer comprises the following steps:
Step (1), adding methacrylic acid-2-isocyanic acid ethyl ester and 3-dimethylamino-1-propanol into a 1, 4-dioxane solvent to react in a nitrogen atmosphere to obtain methacrylic acid-2-carbamate propyl tertiary amine;
Step (2) adding methacrylic acid-2-carbamate propyl tertiary amine and bromoalkyl compound into isopropanol, and carrying out reflux reaction for 60-72h at the temperature of 80-85 ℃ to obtain methacrylic acid-2-carbamate quaternary ammonium salt monomer;
The mass of the methacrylic acid-2-carbamate quaternary ammonium salt and the azodiisobutyronitrile are respectively 15-40% and 0.9-1.2% of that of the acrylonitrile; the copolymerization is carried out for 3-6 hours at the temperature of 70-85 ℃;
the mass of the 3-dimethylamino-1-propanol in the step (1) is 68-82% of the mass of the ethyl methacrylate-2-isocyanate; the reaction in the step (1) is carried out at a temperature of 60-80 ℃ for 3-5h.
2. The antimicrobial acrylic fiber according to claim 1, wherein the mass of the brominated alkyl compound in step (2) is 160-200% of the mass of the 2-urethane propyl tertiary amine methacrylate; the bromoalkyl compound is any one of 1-bromododecane, 1-bromotridecane, 1-bromotetradecane, 1-bromopentadecane and 1-bromohexadecane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410946119.1A CN118547388B (en) | 2024-05-22 | 2024-05-22 | Antibacterial acrylic fiber |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410946119.1A CN118547388B (en) | 2024-05-22 | 2024-05-22 | Antibacterial acrylic fiber |
| CN202410634389.9A CN118207652B (en) | 2024-05-22 | 2024-05-22 | High-strength antibacterial acrylic fiber and preparation process thereof |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410634389.9A Division CN118207652B (en) | 2024-05-22 | 2024-05-22 | High-strength antibacterial acrylic fiber and preparation process thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN118547388A CN118547388A (en) | 2024-08-27 |
| CN118547388B true CN118547388B (en) | 2024-10-18 |
Family
ID=91454943
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410946119.1A Active CN118547388B (en) | 2024-05-22 | 2024-05-22 | Antibacterial acrylic fiber |
| CN202410634389.9A Active CN118207652B (en) | 2024-05-22 | 2024-05-22 | High-strength antibacterial acrylic fiber and preparation process thereof |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410634389.9A Active CN118207652B (en) | 2024-05-22 | 2024-05-22 | High-strength antibacterial acrylic fiber and preparation process thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN118547388B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101153068A (en) * | 2007-09-11 | 2008-04-02 | 东华大学 | Functionalized polyacrylonitrile resin and its preparation and application in fiber |
| CN109135232A (en) * | 2017-06-27 | 2019-01-04 | 江南大学 | A kind of antimicrobial macromolecule composite material and preparation method |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0586575A (en) * | 1991-09-24 | 1993-04-06 | Toyobo Co Ltd | Antimicrobially active acrylic fiber |
| JP5950392B2 (en) * | 2012-06-26 | 2016-07-13 | 関西ペイント株式会社 | Water-based paint composition |
| CN110818864B (en) * | 2019-11-20 | 2023-01-10 | 敏锐生物科技(上海)有限公司 | Preparation method of high-molecular antibacterial agent for improving antibacterial effect |
| CN114163591B (en) * | 2021-11-29 | 2023-08-01 | 南方医科大学 | A kind of block copolymer, block copolymer drug-loaded micelle and its preparation method and application |
| CN115161795B (en) * | 2022-07-11 | 2023-07-04 | 宁波奉化帆盛嘉业服饰有限公司 | Antibacterial fabric and preparation process thereof |
| CN115652460A (en) * | 2022-10-19 | 2023-01-31 | 湖北楼高信息科技有限公司 | Polyacrylonitrile fibre containing guanidyl antiseptic and its preparation method |
-
2024
- 2024-05-22 CN CN202410946119.1A patent/CN118547388B/en active Active
- 2024-05-22 CN CN202410634389.9A patent/CN118207652B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101153068A (en) * | 2007-09-11 | 2008-04-02 | 东华大学 | Functionalized polyacrylonitrile resin and its preparation and application in fiber |
| CN109135232A (en) * | 2017-06-27 | 2019-01-04 | 江南大学 | A kind of antimicrobial macromolecule composite material and preparation method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN118207652B (en) | 2024-08-02 |
| CN118547388A (en) | 2024-08-27 |
| CN118207652A (en) | 2024-06-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US9212301B2 (en) | Composition for preparing polysaccharide fibers | |
| US9334584B2 (en) | Process for preparing polysaccharide fibers from aqueous alkali metal hydroxide solution | |
| JP2016537464A (en) | Composition for producing polysaccharide fibers | |
| CN103233291B (en) | Preparation method of moisture-absorption polyacrylonitrile fiber | |
| CN117385499B (en) | Preparation process of polyurethane-nylon composite fiber material | |
| CN118127663B (en) | Method for preparing flame-retardant DTY polyester yarns by regenerating polyester fibers | |
| CN115233333A (en) | Antibacterial modified polyamide composite fiber and synthetic method thereof | |
| CN118547388B (en) | Antibacterial acrylic fiber | |
| US4377648A (en) | Cellulose-polyacrylonitrile-DMSO-formaldehyde solutions, articles, and methods of making same | |
| CN114672913A (en) | Environment-friendly antibacterial textile fabric and processing technology thereof | |
| CN110952156A (en) | Preparation method of antibacterial and antifouling polyester composite fiber | |
| CN112127013A (en) | A copper ion complexed poly-gamma glutamic acid/chitosan/cotton blended antibacterial knitted fabric and preparation method thereof | |
| US3198764A (en) | Bacteriostatic compositions of acrylonitrile polymers and 2, 2'-thiobis | |
| Wang et al. | Durably and intrinsically antibacterial polyamide 6 (PA6) via backbone end-capping with high temperature-resistant imidazolium | |
| CN118087074A (en) | Antibacterial polyester fiber and preparation method thereof | |
| US3194862A (en) | Acrylonitrile spinning solutions and method of producing filaments therefrom | |
| US2927841A (en) | Process for spinning polyamides which contain a phenylphosphinate and product | |
| CN103205823B (en) | Preparation method of hydrophilic polyacrylonitrile fiber | |
| DE69009337T2 (en) | Polyamide composition. | |
| CN111020734A (en) | A kind of preparation method of long-acting antibacterial polyester fiber | |
| CN117888227B (en) | Preparation method of collagen-containing antibacterial fiber applied to cosmetic brush hair | |
| CN111809268A (en) | Processing method of long-acting antibacterial nylon yarn | |
| CN118422367A (en) | Spinning process of furyl polyamide fibers | |
| DE69117200T2 (en) | Polyamide monofilament | |
| CN116376269B (en) | Antibacterial nylon material and preparation method and application thereof |
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 |