CN113481625A - Preparation method of graphene polylactic acid bi-component composite fiber - Google Patents

Preparation method of graphene polylactic acid bi-component composite fiber Download PDF

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CN113481625A
CN113481625A CN202110966064.7A CN202110966064A CN113481625A CN 113481625 A CN113481625 A CN 113481625A CN 202110966064 A CN202110966064 A CN 202110966064A CN 113481625 A CN113481625 A CN 113481625A
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polylactic acid
component
treated
graphene
composite fiber
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郭松华
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Guangdong Jusheng New Material Technology Co ltd
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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
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • 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
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/06—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from hydroxycarboxylic acids
    • C08G63/08—Lactones or lactides
    • 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
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/91—Polymers modified by chemical after-treatment
    • C08G63/912—Polymers modified by chemical after-treatment derived from hydroxycarboxylic acids
    • 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

Abstract

The invention discloses a preparation method of graphene polylactic acid bi-component composite fibers, and belongs to the field of textiles. The method comprises the following steps: s01, treating polylactic acid with hydrochloric acid; (ii) the treated polylactic acid obtained in S02, S01 is treated with pyridine and a-bromopropionyl bromide; (ii) the treated polylactic acid obtained in S03, S02 is treated with CuBr, 2-bipyridine and vinyl pyrrolidone; s04, drying the treated polylactic acid obtained in S02 to obtain a component A; adding graphene into the component A to obtain a component B; and S05, taking the component A and the component B, and carrying out melt spinning to obtain the graphene polylactic acid bi-component composite fiber. The fabric prepared by the preparation method of the graphene polylactic acid bi-component composite fiber has certain antibacterial capacity.

Description

Preparation method of graphene polylactic acid bi-component composite fiber
Technical Field
The invention belongs to the technical field of textiles, and particularly relates to a preparation method of a graphene polylactic acid bi-component composite fiber.
Background
Polylactic acid, also known as polylactide, is a polyester polymer obtained by polymerizing lactic acid as a main raw material, and is a novel biodegradable material. The polylactic acid has excellent biocompatibility, skin-friendly property and softness, and the processed fabric is mild, smooth and good in drapability.
Graphene is the thinnest, highest-strength, and strongest novel nanomaterial of electric conduction and heat conduction in nature, and has been widely applied to various fields such as semiconductors, electronics, battery energy, aerospace, and the like. The graphene fiber can also enable the composite material to have excellent mechanical, electrical, thermal, radiation-resistant, antibacterial and other functional performances, and can be widely applied to the fields of the graphene cellulose functional composite fiber and corresponding textile products, namely superconducting heat-conducting clothing materials, antibacterial medical materials, biomedical textiles, flame-retardant materials and the like.
CN109487352A discloses a preparation method of graphene polylactic acid bi-component composite fiber. Respectively drying 60-75 wt% of polylactic acid slices and 25-40 wt% of graphene master batches, and mixing to obtain a component A; drying the polylactic acid slices to obtain a component B; respectively melting and extruding the component A and the component B, and then jointly spinning.
Disclosure of Invention
The invention researches the influence of polylactic acid modification on the antibacterial performance of the graphene polylactic acid bi-component composite fiber, and the patent is based on the research.
The invention discloses a preparation method of graphene polylactic acid bi-component composite fiber, which comprises the following steps:
s01, treating polylactic acid with hydrochloric acid;
(ii) the treated polylactic acid obtained in S02, S01 is treated with pyridine and a-bromopropionyl bromide;
(ii) the treated polylactic acid obtained in S03, S02 is treated with CuBr, 2-bipyridine and vinyl pyrrolidone;
s04, drying the treated polylactic acid obtained in S02 to obtain a component A; adding graphene into the component A to obtain a component B;
and S05, taking the component A and the component B, and carrying out melt spinning to obtain the graphene polylactic acid bi-component composite fiber.
In some preferred embodiments of the present invention, in S01, the polylactic acid is soaked with 0.1mol/l HCl solution at 40-60 ℃ for 12-36 h.
In some preferred embodiments of the present invention, the S01 treated polylactic acid is treated with pyridine and a-bromopropionyl bromide at 25-30 ℃ for 12-24h in S02.
In some preferred embodiments of the present invention, in S02, pyridine and a-bromopropionyl bromide are added to the S01-treated polylactic acid in an amount such that the molar ratio of the hydroxyl groups of the polylactic acid to the pyridine and the a-bromopropionyl bromide, based on the hydroxyl groups of the polylactic acid, is 1 (0.5-1): (2-4).
In some further preferred embodiments of the present invention, in S02, the amounts of pyridine and a-bromopropionyl bromide added to the S01-treated polylactic acid are such that the molar ratio of the hydroxyl groups of the polylactic acid to the pyridine and the a-bromopropionyl bromide, based on the hydroxyl groups of the polylactic acid, is 1: 0.5: (2.5-3.5).
In some preferred embodiments of the present invention, in S03, the S02 treated polylactic acid is treated with CuBr, 2-bipyridine and vinyl pyrrolidone at 25-30 ℃ for 36-48 h.
In some preferred embodiments of the invention, in S03, CuBr, 2-bipyridine and vinyl pyrrolidone are added to the S02-treated polylactic acid in a molar ratio of 1:1 to (0.5-1) to (35-60) of bromine groups of polylactic acid to CuBr, 2-bipyridine and vinyl pyrrolidone, based on bromine groups of polylactic acid.
In some further preferred embodiments of the present invention, in S03, CuBr, 2-bipyridine and vinyl pyrrolidone are added to the S02 treated polylactic acid in a molar ratio of 1:0.5 (45-55) of bromine polylactic acid to CuBr, 2-bipyridine and vinyl pyrrolidone, based on bromine polylactic acid.
In some preferred embodiments of the present invention, in S04, component a is added with graphene in a weight ratio of (1.8-2.2):1 to obtain component B.
In some preferred embodiments of the present invention, in S05, the melt spinning, component A and component B are 1 (0.5-1.5) weight ratio, and melt extrusion granulation is performed at 200-220 ℃ to obtain a blend, and the blend is melt spun at a spinning temperature of 180-210 ℃, a winding speed of 80-120m/min, a hot-drawing temperature of 90-110 ℃ and a draw ratio of 1.5-2.5 times to obtain a bicomponent composite fiber with a linear density of 8-12 dtex.
In some preferred embodiments of the present invention, there is further included the step of evaluating the homogeneity of the melt granulation of component a and component B:
s11, determining the initial melting temperature, taking 5 samples, measuring the weight of the unit volume, and recording as a vector X1;
s12, increasing the melting temperature by 10 ℃, taking 5 samples, measuring the weight of the unit volume, and recording as a vector X2;
s13, calculating the homogeneity of X1 and X2 by:
Figure BDA0003223980080000041
Figure BDA0003223980080000042
Figure BDA0003223980080000043
Figure BDA0003223980080000044
if both t1 and t2 are greater than-1.39, the melt granulation is carried out at the initial temperature, and mixing is carried out, otherwise S11 and S12 are repeated until both t1 and t2 are greater than-1.39.
In the invention, the room temperature is 25 +/-1 ℃.
The invention has the beneficial effects that:
(1) the fabric obtained by the preparation method of the graphene polylactic acid bi-component composite fiber has a certain antibacterial capacity;
(2) in the research of the preparation method of the graphene polylactic acid bi-component composite fiber, the modification of polylactic acid in two steps of treating the polylactic acid treated by hydrochloric acid by pyridine and a-bromopropionyl bromide and treating the polylactic acid by CuBr, 2-bipyridine and vinyl pyrrolidone is found to remarkably improve antibacterial performance, and the two steps have mutual support effect.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
In the melt spinning, the component A and the component B are in a weight ratio of 1:1, the mixture is obtained by melt extrusion granulation at 200 ℃ to obtain a blend, and the melt spinning is carried out at the spinning temperature of 190 ℃, the winding speed of 100m/min, the hot drafting temperature of 100 ℃ and the drafting ratio of 2 times to obtain the bicomponent composite fiber with the linear density of 8-10 dtex.
Unless otherwise specified, the examples and comparative examples are parallel tests with the same components, component contents, preparation steps, preparation parameters.
Example 1
The preparation method of the graphene polylactic acid bi-component composite fiber comprises the following steps:
(1) taking polylactic acid, soaking the polylactic acid for 24 hours at 50 ℃ by using 0.1mol/l HCl solution, centrifuging, washing with water and drying;
(2) taking 1g of polylactic acid treated in the step (1), adding pyridine, a-bromopropionyl bromide and 100ml of acetic acid, treating for 24 hours at room temperature in a nitrogen atmosphere, centrifuging, washing with water and drying;
wherein, the molar ratio of the polylactic acid hydroxyl to the pyridine to the a-bromopropionyl bromide is 1: 2;
(3) adding CuBr, 2-bipyridine, vinyl pyrrolidone and 100ml of acetic acid into the polylactic acid treated in the step (2), treating at room temperature for 48 hours in a nitrogen atmosphere, centrifuging, washing with ethanol, and drying;
wherein, the molar ratio of the poly (lactic acid) bromine radical to the CuBr, the 2, 2-bipyridine and the vinyl pyrrolidone is 1:40 in terms of the poly (lactic acid) bromine radical;
(4) drying the polylactic acid treated in the step (3) to obtain a component A; the component A is added with graphene according to the weight ratio of 2:1 to obtain a component B;
(5) and melting and spinning the component A and the component B to obtain the graphene polylactic acid bi-component composite fiber.
Example 2
The preparation method of the graphene polylactic acid bi-component composite fiber comprises the following steps:
(1) taking polylactic acid, soaking the polylactic acid for 12 hours at 60 ℃ by using 0.1mol/l HCl solution, centrifuging, washing with water and drying;
(2) taking 1g of polylactic acid treated in the step (1), adding pyridine, a-bromopropionyl bromide and 100ml of acetic acid, treating for 12h at 30 ℃ in a nitrogen atmosphere, centrifuging, washing with water and drying;
wherein, the molar ratio of the polylactic acid hydroxyl to the pyridine to the a-bromopropionyl bromide is 1: 2.5;
(3) adding CuBr, 2-bipyridine, vinyl pyrrolidone and 100ml of acetic acid into the polylactic acid treated in the step (2), treating for 36 hours at 30 ℃ in a nitrogen atmosphere, centrifuging, washing with ethanol, and drying;
wherein, the molar ratio of the poly (lactic acid) bromine radical to the CuBr, the 2, 2-bipyridine and the vinyl pyrrolidone is 1:40 in terms of the poly (lactic acid) bromine radical;
(4) drying the polylactic acid treated in the step (3) to obtain a component A; the component A is added with graphene according to the weight ratio of 2.2:1 to obtain a component B;
(5) and melting and spinning the component A and the component B to obtain the graphene polylactic acid bi-component composite fiber.
Example 3
The preparation method of the graphene polylactic acid bi-component composite fiber comprises the following steps:
(1) taking polylactic acid, soaking the polylactic acid for 36 hours at 40 ℃ by using 0.1mol/l HCl solution, centrifuging, washing with water, and drying;
(2) taking 1g of polylactic acid treated in the step (1), adding pyridine, a-bromopropionyl bromide and 100ml of acetic acid, treating for 20 hours at room temperature in a nitrogen atmosphere, centrifuging, washing with water and drying;
wherein, the molar ratio of the polylactic acid hydroxyl to the pyridine to the a-bromopropionyl bromide is 1: 2;
(3) adding CuBr, 2-bipyridine, vinyl pyrrolidone and 100ml of acetic acid into the polylactic acid treated in the step (2), treating at room temperature for 46 hours in a nitrogen atmosphere, centrifuging, washing with ethanol, and drying;
wherein, calculated by polylactic acid bromine radical, the molar ratio of the polylactic acid bromine radical to the CuBr, the 2, 2-bipyridine and the vinyl pyrrolidone is 1: 35;
(4) drying the polylactic acid treated in the step (3) to obtain a component A; the component A is added with graphene according to the weight ratio of 1.8:1 to obtain a component B;
(5) and melting and spinning the component A and the component B to obtain the graphene polylactic acid bi-component composite fiber.
Example 4
The preparation method of the graphene polylactic acid bi-component composite fiber comprises the following steps:
(1) taking polylactic acid, soaking the polylactic acid for 24 hours at 50 ℃ by using 0.1mol/l HCl solution, centrifuging, washing with water and drying;
(2) taking 1g of polylactic acid treated in the step (1), adding pyridine, a-bromopropionyl bromide and 100ml of acetic acid, treating for 24 hours at room temperature in a nitrogen atmosphere, centrifuging, washing with water and drying;
wherein, the molar ratio of the polylactic acid hydroxyl to the pyridine to the a-bromopropionyl bromide is 1: 0.5: 3;
(3) adding CuBr, 2-bipyridine, vinyl pyrrolidone and 100ml of acetic acid into the polylactic acid treated in the step (2), treating at room temperature for 48 hours in a nitrogen atmosphere, centrifuging, washing with ethanol, and drying;
wherein, calculated by polylactic acid bromine radical, the molar ratio of the polylactic acid bromine radical to the CuBr, the 2, 2-bipyridine and the vinyl pyrrolidone is 1: 0.5: 1: 50;
(4) drying the polylactic acid treated in the step (3) to obtain a component A; the component A is added with graphene according to the weight ratio of 2:1 to obtain a component B;
(5) and melting and spinning the component A and the component B to obtain the graphene polylactic acid bi-component composite fiber.
Example 5
The preparation method of the graphene polylactic acid bi-component composite fiber comprises the following steps:
(1) taking polylactic acid, soaking the polylactic acid for 24 hours at 50 ℃ by using 0.1mol/l HCl solution, centrifuging, washing with water and drying;
(2) taking 1g of polylactic acid treated in the step (1), adding pyridine, a-bromopropionyl bromide and 100ml of acetic acid, treating for 24 hours at room temperature in a nitrogen atmosphere, centrifuging, washing with water and drying;
wherein, the molar ratio of the polylactic acid hydroxyl to the pyridine to the a-bromopropionyl bromide is 1: 0.5: 4;
(3) adding CuBr, 2-bipyridine, vinyl pyrrolidone and 100ml of acetic acid into the polylactic acid treated in the step (2), treating at room temperature for 48 hours in a nitrogen atmosphere, centrifuging, washing with ethanol, and drying;
wherein, calculated by polylactic acid bromine radical, the molar ratio of the polylactic acid bromine radical to the CuBr, the 2, 2-bipyridine and the vinyl pyrrolidone is 1: 0.5: 1: 60;
(4) drying the polylactic acid treated in the step (3) to obtain a component A; the component A is added with graphene according to the weight ratio of 2:1 to obtain a component B;
(5) and melting and spinning the component A and the component B to obtain the graphene polylactic acid bi-component composite fiber.
Example 6
The preparation method of the graphene polylactic acid bi-component composite fiber is different from the embodiment 1 in that the preparation method further comprises the following steps of evaluating the uniformity of melt granulation of the component A and the component B:
s11, determining the initial melting temperature, taking 5 samples, measuring the weight of the unit volume, and recording as a vector X1;
s12, increasing the melting temperature by 10 ℃, taking 5 samples, measuring the weight of the unit volume, and recording as a vector X2;
s13, calculating the homogeneity of X1 and X2 by:
Figure BDA0003223980080000101
Figure BDA0003223980080000102
Figure BDA0003223980080000103
Figure BDA0003223980080000104
if both t1 and t2 are greater than-1.39, the melt granulation is carried out at the initial temperature, and mixing is carried out, otherwise S11 and S12 are repeated until both t1 and t2 are greater than-1.39.
By the method of this example, the temperature at which the components A and B are sufficiently melted in the melt granulation can be rapidly determined.
Comparative example 1
The preparation method of the graphene polylactic acid bi-component composite fiber is different from the preparation method of the graphene polylactic acid bi-component composite fiber in example 1 in that the step (3) is omitted.
Comparative example 2
The preparation method of the graphene polylactic acid bi-component composite fiber is different from the preparation method of the graphene polylactic acid bi-component composite fiber in example 1 in that the step (2) is omitted. In step (3), CuBr, 2-bipyridine and vinyl pyrrolidone were added in the same amounts by weight as in example 1.
Performance inspection
The graphene polylactic acid bi-component composite fibers of the examples and the comparative examples are spun in the same manner, woven into fabric, repeatedly washed for 30 times, soaked in tap water for 10min, washed by a washing machine for 10min, and dried at 60 ℃ for 10 min. The antibacterial rate of the fabric is tested according to the method of evaluation of antibacterial performance of textiles (part 3) namely oscillation method (GB/T20944.3-2008).
Table 1 bacteriostatic situation of graphene polylactic acid bi-component composite fiber fabric
Figure BDA0003223980080000111
Figure BDA0003223980080000121
In the same column of data, marked with different lower case letters to represent significant difference, P is less than 0.05
The results show that the fabrics woven by the graphene polylactic acid bi-component composite fibers obtained in the examples 1-5 have certain antibacterial capability which is obviously superior to that of the comparative examples 1 and 2; in examples 1 to 5, example 4 was significantly superior in antibacterial ability to examples 1 to 3 and 5.
While the preferred embodiments and examples of the present invention have been described in detail, the present invention is not limited to the embodiments and examples, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.

Claims (10)

1. The preparation method of the graphene polylactic acid bi-component composite fiber is characterized by comprising the following steps:
s01, treating polylactic acid with hydrochloric acid;
(ii) the treated polylactic acid obtained in S02, S01 is treated with pyridine and a-bromopropionyl bromide;
(ii) the treated polylactic acid obtained in S03, S02 is treated with CuBr, 2-bipyridine and vinyl pyrrolidone;
s04, drying the treated polylactic acid obtained in S02 to obtain a component A; adding graphene into the component A to obtain a component B;
and S05, taking the component A and the component B, and carrying out melt spinning to obtain the graphene polylactic acid bi-component composite fiber.
2. The method according to claim 1, wherein in S01, the polylactic acid is soaked in 0.1mol/l HCl solution at 40-60 ℃ for 12-36 h.
3. The method according to claim 1 or 2, wherein the polylactic acid treated in S02 with S01 is treated with pyridine and a-bromopropionyl bromide at 25-30 ℃ for 12-24 h.
4. The process according to any one of claims 1 to 3, wherein the amount of pyridine and a-bromopropionyl bromide added to the polylactic acid treated in S01 in S02 is such that the molar ratio of the hydroxyl group of the polylactic acid to the pyridine and the a-bromopropionyl bromide based on the hydroxyl group of the polylactic acid is 1 (0.5 to 1): (2-4).
5. The process according to any one of claims 1 to 4, wherein in S02, pyridine and a-bromopropionyl bromide are added to the S01-treated polylactic acid in an amount such that the molar ratio of the hydroxyl group of the polylactic acid to the pyridine and the a-bromopropionyl bromide based on the hydroxyl group of the polylactic acid is 1: 0.5: (2.5-3.5).
6. The method according to any one of claims 1 to 5, wherein the polylactic acid treated with S02 in S03 is treated with CuBr, 2-bipyridine and vinyl pyrrolidone at 25 to 30 ℃ for 36 to 48 hours.
7. The process according to any one of claims 1 to 6, wherein in S03, CuBr, 2-bipyridine and vinyl pyrrolidone are added to the S02-treated polylactic acid in a molar ratio of 1:1 (0.5-1) to 1: (35-60).
8. The process according to any one of claims 1 to 7, wherein in S03, CuBr, 2-bipyridine and vinyl pyrrolidone are added to the S02-treated polylactic acid in a molar ratio of the bromine group of the polylactic acid to the CuBr, 2-bipyridine and vinyl pyrrolidone, based on the bromine group of the polylactic acid, of 1: 0.5: 1: (45-55).
9. The method according to any one of claims 1 to 8, wherein in S04, graphene is added to component A in a weight ratio of (1.8-2.2) to 1 to obtain component B.
10. The method according to any one of claims 1 to 9, wherein in S05, the melt-spun, component A and component B are 1 (0.5-1.5) by weight ratio, and melt-extruded and pelletized at 200-220 ℃ to obtain a blend, and the blend is melt-spun at a spinning temperature of 180-210 ℃, a winding speed of 80-120m/min, a hot-drawing temperature of 90-110 ℃ and a draw ratio of 1.5-2.5 times to obtain a bicomponent composite fiber filament with a linear density of 8-12 dtex.
CN202110966064.7A 2021-08-23 2021-08-23 Preparation method of graphene polylactic acid bi-component composite fiber Withdrawn CN113481625A (en)

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Application publication date: 20211008