CN117265694A - Method for preparing bio-based PTT fiber by recycling waste fabric - Google Patents

Method for preparing bio-based PTT fiber by recycling waste fabric Download PDF

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CN117265694A
CN117265694A CN202311549429.1A CN202311549429A CN117265694A CN 117265694 A CN117265694 A CN 117265694A CN 202311549429 A CN202311549429 A CN 202311549429A CN 117265694 A CN117265694 A CN 117265694A
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ptt fiber
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ptt
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CN117265694B (en
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王霄
藤冠强
苗莉
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Shanghai Huahao Chemical 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
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J11/00—Recovery or working-up of waste materials
    • C08J11/04—Recovery or working-up of waste materials of polymers
    • C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
    • C08J11/18—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material
    • C08J11/22—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic oxygen-containing compounds
    • C08J11/24—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic oxygen-containing compounds containing hydroxyl groups
    • 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
    • D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
    • 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
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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  • Organic Chemistry (AREA)
  • Artificial Filaments (AREA)

Abstract

The invention discloses a method for preparing bio-based PTT fibers by recycling waste fabrics, and relates to the field of fibers. In the preparation of the bio-based PTT fiber, the waste PTT fabric is subjected to alcoholysis to prepare the PTT fiber oligomer; reacting chitosan with acrolein to obtain vinyl chitosan; PTT fiber oligomer reacts with dimethyl phosphite to prepare PTT fiber master batch; mixing PTT fiber master batch with vinyl chitosan, kong Ji alkene and solvent methylene dichloride, and preparing porous PTT fibers through electrostatic spinning; reacting the porous PTT fiber with methyl laurate to obtain the bio-based PTT fiber. The bio-based PTT fiber prepared by the invention has excellent mechanical property, flame retardance, hygroscopicity and washability.

Description

Method for preparing bio-based PTT fiber by recycling waste fabric
Technical Field
The invention relates to the technical field of fibers, in particular to a method for preparing bio-based PTT fibers by recycling waste fabrics.
Background
The PTT fiber is polymerized by using 1,3 propanediol and terephthalic acid as raw materials, is a novel polyester fiber which integrates the advantages of excellent rebound resilience, stain resistance, wear resistance, spinnability, dyeing property, soft hand feeling and the like, and can be widely applied to the clothing fields of sportswear, underwear and the like. With the rapid development of human society, a large number of waste textiles are generated, and the problem of waste treatment in production and after consumption is not neglected while the fiber fabric brings convenience to life of people. Although polyester fibers do not produce substances which are toxic to nature after entering the natural environment, the chemical inertness of the polyester fibers makes the polyester fibers difficult to degrade by air and microorganisms, and the polyester fibers occupy a large amount of space if not subjected to recycling treatment. In addition, raw materials for synthesizing the polyester fibers are derived from petroleum, and it is well known that petroleum is a limited natural resource, and if a large amount of waste is not recycled, the environment is threatened, and the resource is wasted.
Because PTT molecular chains are orderly arranged, have high crystallinity and lack hydrophilic groups, the PTT molecular chains have poor hygroscopicity, are easy to generate smoky feeling in the wearing process, reduce the comfort of clothing, and the PTT fiber belongs to inflammable materials like other polyester fibers, and has lower mechanical strength than PET. Therefore, there is a need to modify PTT fibers to provide good hygroscopicity and flame retardancy.
Disclosure of Invention
The invention aims to provide a method for preparing bio-based PTT fiber by recycling waste fabrics, which solves the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
the method for preparing the bio-based PTT fiber by recycling the waste fabric comprises the steps of reacting PTT fiber oligomer with dimethyl phosphite to prepare PTT fiber master batch; mixing PTT fiber master batch with vinyl chitosan, a pore-forming agent and methylene dichloride, and preparing porous PTT fibers through electrostatic spinning; and then reacting the porous PTT fiber with methyl laurate.
As optimization, the PTT fiber oligomer is prepared by alcoholysis of waste PTT fabric with 1, 3-propanediol.
Preferably, the vinyl chitosan is prepared by reacting chitosan with acrolein.
Preferably, the porogen is camphene.
As an optimization, the following preparation steps are included:
(1) Immersing waste PTT fabric into pure water for ultrasonic treatment for 2 hours, taking out, drying at 70-80 ℃ for 4-6 hours, crushing into PTT chips with the particle size smaller than 0.5mm by using a wall breaking machine, and mixing the PTT chips, 1, 3-propanediol and zinc acetate according to the mass ratio of 1:3: (0.01-0.03), stirring and refluxing for 1-2 hours at 200-210 ℃ and 600-800 r/min in a nitrogen atmosphere, cooling to 80-90 ℃, carrying out suction filtration with deionized water for 3-5 times to obtain filtrate, standing the filtrate at 0-2 ℃ for 24-36 hours, filtering, and drying at 70-80 ℃ for 5-6 hours to obtain PTT fiber oligomer;
(2) Chitosan, acetic acid and formaldehyde are mixed according to the mass ratio of 1: (2-3): (24-26) uniformly mixing, stirring at 20-30 ℃ for 1-2 hours at 300-500 r/min, adding acrolein with the mass 2-3 times of that of chitosan, stirring and refluxing at 50-60 ℃ for 8-10 hours at 300-500 r/min, drying at 5-10 Pa and 50-60 ℃ for 3-4 hours, washing with absolute ethyl alcohol for 3-5 times, and drying at 5-10 Pa and 50-60 ℃ for 4-6 hours to obtain vinyl chitosan;
(3) The PTT fiber oligomer, the dimethyl phosphite, the sodium hydroxide and the toluene are mixed according to the mass ratio of 1: (1-1.2): (0.03 to 0.05): (8-10) uniformly mixing, stirring and reacting for 3-4 hours at the temperature of 240-270 ℃ and the speed of 400-600 r/min under the nitrogen atmosphere, washing for 3-5 times by deionized water, drying for 7-8 hours at the temperature of 30-40 ℃ under the pressure of 5-10 Pa to obtain PTT fiber master batch, and mixing PTT fiber master batch, vinyl chitosan, azodiisobutyronitrile, camphene and methylene dichloride according to the mass ratio of 1: (0.5 to 0.7): (0.03 to 0.05): (0.1 to 0.2): (8-10) uniformly mixing, stirring for 8-10 hours at 20-30 ℃ at 400-600 r/min to prepare a fiber spinning solution, filling the fiber spinning solution into a micropump, adopting an ice plate covered with aluminum foil as a receiving device, adjusting the receiving distance to be 16-18 cm, controlling the voltage to be 23-25 kV in the spinning process, controlling the advancing rate to be 0.6-0.7 mL/h, controlling the environmental temperature to be 20-30 ℃ and the spinning humidity to be 50% -60%, and performing electrospinning in an electrospinning device to prepare a primary PTT fiber, and drying the primary PTT fiber at 70-80 ℃ for 5-6 hours to prepare the porous PTT fiber;
(4) The porous PTT fiber, methyl laurate and n-hexane are mixed according to the mass ratio of 1: (1-1.2): (8-10), uniformly mixing, stirring at 70-80 ℃ for reaction for 3-5 hours at 300-500 r/min, taking out, washing with absolute ethyl alcohol for 3-5 times, and drying at 70-80 ℃ for 4-6 hours to obtain the bio-based PTT fiber.
As optimization, the alcoholysis reaction process of the waste PTT fabric in the step (1) is as follows:
。
as an optimization, the reaction process of the vinyl chitosan in the step (2) is as follows:
。
as an optimization, the reaction process of the porous PTT fiber in the step (3) is as follows:
。
compared with the prior art, the invention has the following advantages:
in the preparation of the bio-based PTT fiber, the waste PTT fabric is subjected to alcoholysis to prepare the PTT fiber oligomer; reacting chitosan with acrolein to obtain vinyl chitosan; PTT fiber oligomer reacts with dimethyl phosphite to prepare PTT fiber master batch; mixing PTT fiber master batch with vinyl chitosan, kong Ji alkene and solvent methylene dichloride, preparing porous PTT fiber through electrostatic spinning, and then reacting the porous PTT fiber with methyl laurate;
firstly, carrying out alcoholysis on waste PTT fabric by using 1, 3-propanediol to prepare PTT fiber oligomer; carrying out Schiff base reaction on chitosan and acrolein, and introducing double bonds into a chitosan molecular chain to prepare vinyl chitosan; the PTT fiber master batch is prepared by transesterification of PTT fiber oligomer and dimethyl phosphite, and the introduction of the dimethyl phosphite endows the PTT fiber master batch with flame retardant property; uniformly mixing PTT fiber master batch with vinyl chitosan, kong Ji alkene and solvent methylene dichloride, preparing a primary PTT fiber through electrostatic spinning, heating and drying the primary PTT fiber to sublimate Kong Ji alkene, volatilizing the solvent methylene dichloride, forming a porous structure on the primary fiber, improving the specific surface area of the primary PTT fiber, heating and drying to cause P-H bonds on the primary PTT fiber to generate phosphine addition with double bonds on the vinyl chitosan to form a crosslinked structure, preparing a porous PTT fiber, endowing the porous PTT fiber with excellent mechanical property, and simultaneously, endowing the porous PTT fiber with excellent moisture absorption property through the synergistic effect of the porous structure in the porous PTT fiber and hydrophilic groups on the chitosan;
secondly, performing transesterification reaction on the porous PTT fiber and methyl laurate in normal hexane to obtain a bio-based PTT fiber; hydroxyl on the surface of the porous PTT fiber is converted into a long carbon chain through transesterification, so that the washing resistance of the porous PTT fiber is improved; n-hexane is a hydrophobic solvent, and the porous PTT fiber has hydrophilicity, and n-hexane is used as a reaction solvent, so that methyl laurate can only react hydroxyl groups on the surface of the porous PTT fiber, and has no influence on hydroxyl groups in the pores of the porous PTT fiber, and the moisture absorption performance of the porous PTT fiber is not influenced.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, 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.
Example 1: a method for preparing bio-based PTT fiber by recycling waste fabrics comprises the following preparation steps:
(1) Immersing waste PTT fabric into pure water for ultrasonic treatment for 2 hours, taking out, drying at 70 ℃ for 6 hours, crushing into PTT chips with the particle size smaller than 0.5mm by using a wall breaking machine, and mixing the PTT chips, 1, 3-propanediol and zinc acetate according to the mass ratio of 1:3:0.01 is evenly mixed, and is stirred and refluxed for 2 hours at 200 ℃ and 600r/min in nitrogen atmosphere, cooled to 80 ℃, filtered with deionized water for 3 times to obtain filtrate, the filtrate is stood for 36 hours at 0 ℃, filtered and dried for 6 hours at 70 ℃ to obtain PTT fiber oligomer;
(2) Chitosan, acetic acid and formaldehyde are mixed according to the mass ratio of 1:2:24, stirring for 1h at 20 ℃ at 300r/min, adding acrolein with the mass 2 times of that of chitosan, stirring and refluxing for 10h at 50 ℃ at 300r/min, drying for 4h at 5Pa and 50 ℃, washing for 3 times with absolute ethyl alcohol, and drying for 6h at 5Pa and 50 ℃ to obtain vinyl chitosan;
(3) The PTT fiber oligomer, the dimethyl phosphite, the sodium hydroxide and the toluene are mixed according to the mass ratio of 1:1:0.03:8, uniformly mixing, stirring at 240 ℃ at 400r/min under nitrogen atmosphere, reacting for 4 hours, washing with deionized water for 3 times, drying at 5Pa and 30 ℃ for 8 hours to obtain PTT fiber master batch, and mixing PTT fiber master batch, vinyl chitosan, azodiisobutyronitrile, camphene and methylene dichloride according to the mass ratio of 1:0.5:0.03:0.1:8, uniformly mixing, stirring for 10 hours at 20 ℃ and 400r/min to prepare a fiber spinning solution, loading the fiber spinning solution into a micro pump, adopting an ice plate covered with aluminum foil as a receiving device, adjusting the receiving distance to be 16cm, controlling the voltage in the spinning process to be 23 kV, controlling the advancing rate to be 0.6mL/h, controlling the environmental temperature to be 20 ℃ and the spinning humidity to be 50%, and carrying out electrospinning in an electrospinning device to prepare a primary PTT fiber, and drying the primary PTT fiber at 70 ℃ for 6 hours to prepare the porous PTT fiber;
(4) The porous PTT fiber, methyl laurate and n-hexane are mixed according to the mass ratio of 1:1.2:8, uniformly mixing, stirring at 70 ℃ and 300r/min for reaction for 5 hours, taking out, washing with absolute ethyl alcohol for 3 times, and drying at 70 ℃ for 6 hours to obtain the bio-based PTT fiber.
Example 2: a method for preparing bio-based PTT fiber by recycling waste fabrics comprises the following preparation steps:
(1) Immersing waste PTT fabric into pure water for ultrasonic treatment for 2 hours, taking out, drying at 75 ℃ for 5 hours, crushing into PTT chips with the particle size smaller than 0.5mm by using a wall breaking machine, and mixing the PTT chips, 1, 3-propanediol and zinc acetate according to the mass ratio of 1:3:0.02, stirring and refluxing for 1.5 hours at the temperature of 205 ℃ and 700r/min in a nitrogen atmosphere, cooling to the temperature of 85 ℃, carrying out suction filtration with deionized water for 4 times to obtain filtrate, standing the filtrate at the temperature of 1 ℃ for 30 hours, filtering, and drying at the temperature of 75 ℃ for 5.5 hours to obtain PTT fiber oligomer;
(2) Chitosan, acetic acid and formaldehyde are mixed according to the mass ratio of 1:2.5:25, stirring at 25 ℃ at 400r/min for 1.5h, adding acrolein with the mass 2.5 times of that of chitosan, stirring at 55 ℃ at 400r/min for reflux for 9h, drying at 8Pa at 55 ℃ for 3.5h, washing with absolute ethyl alcohol for 4 times, and drying at 8Pa at 55 ℃ for 5h to obtain vinyl chitosan;
(3) The PTT fiber oligomer, the dimethyl phosphite, the sodium hydroxide and the toluene are mixed according to the mass ratio of 1:1.1:0.04:9, uniformly mixing, stirring and reacting for 3.5 hours at 255 ℃ and 500r/min under nitrogen atmosphere, washing for 4 times by using deionized water, drying for 7.5 hours at 8Pa and 35 ℃ to obtain PTT fiber master batch, and mixing PTT fiber master batch, vinyl chitosan, azodiisobutyronitrile, camphene and methylene dichloride according to the mass ratio of 1:0.6:0.04:0.15:9, uniformly mixing, stirring for 9 hours at 25 ℃ and 500r/min to prepare a fiber spinning solution, loading the fiber spinning solution into a micro pump, adopting an ice plate covered with aluminum foil as a receiving device, adjusting the receiving distance to be 17cm, adjusting the voltage in the spinning process to be 24kV, adjusting the propulsion rate to be 0.65mL/h, and performing electrospinning in an electrospinning device at the environment temperature of 25 ℃ and the spinning humidity of 55%, so as to prepare a primary PTT fiber, and drying the primary PTT fiber at 75 ℃ for 5.5 hours to prepare a porous PTT fiber;
(4) The porous PTT fiber, methyl laurate and n-hexane are mixed according to the mass ratio of 1:1.1:9, uniformly mixing, stirring at 75 ℃ for reaction for 4 hours at 400r/min, taking out, washing with absolute ethyl alcohol for 4 times, and drying at 75 ℃ for 5 hours to obtain the bio-based PTT fiber.
Example 3: a method for preparing bio-based PTT fiber by recycling waste fabrics comprises the following preparation steps:
(1) Immersing waste PTT fabric into pure water for ultrasonic treatment for 2 hours, taking out, drying for 4 hours at 80 ℃, crushing into PTT chips with the particle size smaller than 0.5mm by using a wall breaking machine, and mixing the PTT chips, 1, 3-propanediol and zinc acetate according to the mass ratio of 1:3:0.03, stirring and refluxing for 1h at 210 ℃ and 800r/min in a nitrogen atmosphere, cooling to 90 ℃, carrying out suction filtration with deionized water for 5 times to obtain filtrate, standing the filtrate at 2 ℃ for 24h, filtering, and drying at 80 ℃ for 5h to obtain PTT fiber oligomer;
(2) Chitosan, acetic acid and formaldehyde are mixed according to the mass ratio of 1:3:26, uniformly mixing, stirring at 30 ℃ for 2 hours at 500r/min, adding acrolein with the mass 3 times of that of chitosan, stirring at 60 ℃ for reflux at 500r/min for 8 hours, drying at 10Pa and 60 ℃ for 3 hours, washing with absolute ethanol for 5 times, and drying at 10Pa and 60 ℃ for 4 hours to prepare vinyl chitosan;
(3) The PTT fiber oligomer, the dimethyl phosphite, the sodium hydroxide and the toluene are mixed according to the mass ratio of 1:1.2:0.05:10, uniformly mixing, stirring at 270 ℃ and 600r/min under nitrogen atmosphere, reacting for 3 hours, washing with deionized water for 5 times, drying at 10Pa and 40 ℃ for 7 hours to obtain PTT fiber master batch, and mixing PTT fiber master batch, vinyl chitosan, azodiisobutyronitrile, camphene and methylene dichloride according to the mass ratio of 1:0.7:0.05:0.2:10, uniformly mixing, stirring for 8 hours at 30 ℃ at 600r/min to prepare a fiber spinning solution, loading the fiber spinning solution into a micro pump, adopting an ice plate covered with aluminum foil as a receiving device, adjusting the receiving distance to be 18cm, controlling the voltage in the spinning process to be 25 kV, controlling the advancing rate to be 0.7mL/h, controlling the environmental temperature to be 30 ℃ and the spinning humidity to be 60%, and carrying out electrospinning in an electrospinning device to prepare a primary PTT fiber, and drying the primary PTT fiber at 80 ℃ for 5 hours to prepare a porous PTT fiber;
(4) The porous PTT fiber, methyl laurate and n-hexane are mixed according to the mass ratio of 1:1:10, uniformly mixing, stirring at 80 ℃ for reaction for 3 hours at 500r/min, taking out, washing with absolute ethyl alcohol for 5 times, and drying at 80 ℃ for 4 hours to obtain the bio-based PTT fiber.
A method for preparing bio-based PTT fiber by recycling waste fabrics comprises the following preparation steps:
(1) Immersing waste PTT fabric into pure water for ultrasonic treatment for 2 hours, taking out, drying at 75 ℃ for 5 hours, crushing into PTT chips with the particle size smaller than 0.5mm by using a wall breaking machine, and mixing the PTT chips, 1, 3-propanediol and zinc acetate according to the mass ratio of 1:3:0.02, stirring and refluxing for 1.5 hours at the temperature of 205 ℃ and 700r/min in a nitrogen atmosphere, cooling to the temperature of 85 ℃, carrying out suction filtration with deionized water for 4 times to obtain filtrate, standing the filtrate at the temperature of 1 ℃ for 30 hours, filtering, and drying at the temperature of 75 ℃ for 5.5 hours to obtain PTT fiber oligomer;
(2) The PTT fiber oligomer, the dimethyl phosphite, the sodium hydroxide and the toluene are mixed according to the mass ratio of 1:1.1:0.04:9, uniformly mixing, stirring and reacting for 3.5 hours at 255 ℃ and 500r/min under nitrogen atmosphere, washing for 4 times by using deionized water, drying for 7.5 hours at 8Pa and 35 ℃ to obtain PTT fiber master batch, wherein the PTT fiber master batch, chitosan, camphene and methylene dichloride are mixed according to the mass ratio of 1:0.6:0.15:9, uniformly mixing, stirring for 9 hours at 25 ℃ and 500r/min to prepare a fiber spinning solution, loading the fiber spinning solution into a micro pump, adopting an ice plate covered with aluminum foil as a receiving device, adjusting the receiving distance to be 17cm, adjusting the voltage in the spinning process to be 24kV, adjusting the propulsion rate to be 0.65mL/h, and performing electrospinning in an electrospinning device at the environment temperature of 25 ℃ and the spinning humidity of 55%, so as to prepare a primary PTT fiber, and drying the primary PTT fiber at 75 ℃ for 5.5 hours to prepare a porous PTT fiber;
(3) The porous PTT fiber, methyl laurate and n-hexane are mixed according to the mass ratio of 1:1.1:9, uniformly mixing, stirring at 75 ℃ for reaction for 4 hours at 400r/min, taking out, washing with absolute ethyl alcohol for 4 times, and drying at 75 ℃ for 5 hours to obtain the bio-based PTT fiber.
Comparative example 2
A method for preparing bio-based PTT fiber by recycling waste fabrics comprises the following preparation steps:
(1) Immersing waste PTT fabric into pure water for ultrasonic treatment for 2 hours, taking out, drying at 75 ℃ for 5 hours, crushing into PTT chips with the particle size smaller than 0.5mm by using a wall breaking machine, and mixing the PTT chips, 1, 3-propanediol and zinc acetate according to the mass ratio of 1:3:0.02, stirring and refluxing for 1.5 hours at the temperature of 205 ℃ and 700r/min in a nitrogen atmosphere, cooling to the temperature of 85 ℃, carrying out suction filtration with deionized water for 4 times to obtain filtrate, standing the filtrate at the temperature of 1 ℃ for 30 hours, filtering, and drying at the temperature of 75 ℃ for 5.5 hours to obtain PTT fiber oligomer;
(2) Chitosan, acetic acid and formaldehyde are mixed according to the mass ratio of 1:2.5:25, stirring at 25 ℃ at 400r/min for 1.5h, adding acrolein with the mass 2.5 times of that of chitosan, stirring at 55 ℃ at 400r/min for reflux for 9h, drying at 8Pa at 55 ℃ for 3.5h, washing with absolute ethyl alcohol for 4 times, and drying at 8Pa at 55 ℃ for 5h to obtain vinyl chitosan;
(3) The PTT fiber oligomer, sodium hydroxide and toluene are mixed according to the mass ratio of 1:0.04:9, uniformly mixing, stirring and reacting for 3.5 hours at 255 ℃ and 500r/min under nitrogen atmosphere, washing for 4 times by using deionized water, drying for 7.5 hours at 8Pa and 35 ℃ to obtain PTT fiber master batch, and mixing PTT fiber master batch, vinyl chitosan, azodiisobutyronitrile, camphene and methylene dichloride according to the mass ratio of 1:0.6:0.04:0.15:9, uniformly mixing, stirring for 9 hours at 25 ℃ and 500r/min to prepare a fiber spinning solution, loading the fiber spinning solution into a micro pump, adopting an ice plate covered with aluminum foil as a receiving device, adjusting the receiving distance to be 17cm, adjusting the voltage in the spinning process to be 24kV, adjusting the propulsion rate to be 0.65mL/h, and performing electrospinning in an electrospinning device at the environment temperature of 25 ℃ and the spinning humidity of 55%, so as to prepare a primary PTT fiber, and drying the primary PTT fiber at 75 ℃ for 5.5 hours to prepare a porous PTT fiber;
(4) The porous PTT fiber, methyl laurate and n-hexane are mixed according to the mass ratio of 1:1.1:9, uniformly mixing, stirring at 75 ℃ for reaction for 4 hours at 400r/min, taking out, washing with absolute ethyl alcohol for 4 times, and drying at 75 ℃ for 5 hours to obtain the bio-based PTT fiber.
Comparative example 3
A method for preparing bio-based PTT fiber by recycling waste fabrics comprises the following preparation steps:
(1) Immersing waste PTT fabric into pure water for ultrasonic treatment for 2 hours, taking out, drying at 75 ℃ for 5 hours, crushing into PTT chips with the particle size smaller than 0.5mm by using a wall breaking machine, and mixing the PTT chips, 1, 3-propanediol and zinc acetate according to the mass ratio of 1:3:0.02, stirring and refluxing for 1.5 hours at the temperature of 205 ℃ and 700r/min in a nitrogen atmosphere, cooling to the temperature of 85 ℃, carrying out suction filtration with deionized water for 4 times to obtain filtrate, standing the filtrate at the temperature of 1 ℃ for 30 hours, filtering, and drying at the temperature of 75 ℃ for 5.5 hours to obtain PTT fiber oligomer;
(2) Chitosan, acetic acid and formaldehyde are mixed according to the mass ratio of 1:2.5:25, stirring at 25 ℃ at 400r/min for 1.5h, adding acrolein with the mass 2.5 times of that of chitosan, stirring at 55 ℃ at 400r/min for reflux for 9h, drying at 8Pa at 55 ℃ for 3.5h, washing with absolute ethyl alcohol for 4 times, and drying at 8Pa at 55 ℃ for 5h to obtain vinyl chitosan;
(3) The PTT fiber oligomer, the dimethyl phosphite, the sodium hydroxide and the toluene are mixed according to the mass ratio of 1:1.1:0.04:9, uniformly mixing, stirring and reacting for 3.5 hours at 255 ℃ and 500r/min under nitrogen atmosphere, washing for 4 times by using deionized water, drying for 7.5 hours at 8Pa and 35 ℃ to obtain PTT fiber master batch, and mixing the PTT fiber master batch, vinyl chitosan, azodiisobutyronitrile and methylene dichloride according to the mass ratio of 1:0.6:0.15:9, uniformly mixing, stirring for 9 hours at 25 ℃ and 500r/min to prepare a fiber spinning solution, loading the fiber spinning solution into a micro pump, adopting an ice plate covered with aluminum foil as a receiving device, adjusting the receiving distance to be 17cm, adjusting the voltage in the spinning process to be 24kV, adjusting the propulsion rate to be 0.65mL/h, and performing electrospinning in an electrospinning device at the environment temperature of 25 ℃ and the spinning humidity of 55%, so as to prepare a primary PTT fiber, and drying the primary PTT fiber at 75 ℃ for 5.5 hours to prepare a porous PTT fiber;
(4) The porous PTT fiber, methyl laurate and n-hexane are mixed according to the mass ratio of 1:1.1:9, uniformly mixing, stirring at 75 ℃ for reaction for 4 hours at 400r/min, taking out, washing with absolute ethyl alcohol for 4 times, and drying at 75 ℃ for 5 hours to obtain the bio-based PTT fiber.
Comparative example 4
A method for preparing bio-based PTT fiber by recycling waste fabrics comprises the following preparation steps:
(1) Immersing waste PTT fabric into pure water for ultrasonic treatment for 2 hours, taking out, drying at 75 ℃ for 5 hours, crushing into PTT chips with the particle size smaller than 0.5mm by using a wall breaking machine, and mixing the PTT chips, 1, 3-propanediol and zinc acetate according to the mass ratio of 1:3:0.02, stirring and refluxing for 1.5 hours at the temperature of 205 ℃ and 700r/min in a nitrogen atmosphere, cooling to the temperature of 85 ℃, carrying out suction filtration with deionized water for 4 times to obtain filtrate, standing the filtrate at the temperature of 1 ℃ for 30 hours, filtering, and drying at the temperature of 75 ℃ for 5.5 hours to obtain PTT fiber oligomer;
(2) Chitosan, acetic acid and formaldehyde are mixed according to the mass ratio of 1:2.5:25, stirring at 25 ℃ at 400r/min for 1.5h, adding acrolein with the mass 2.5 times of that of chitosan, stirring at 55 ℃ at 400r/min for reflux for 9h, drying at 8Pa at 55 ℃ for 3.5h, washing with absolute ethyl alcohol for 4 times, and drying at 8Pa at 55 ℃ for 5h to obtain vinyl chitosan;
(3) The PTT fiber oligomer, the dimethyl phosphite, the sodium hydroxide and the toluene are mixed according to the mass ratio of 1:1.1:0.04:9, uniformly mixing, stirring and reacting for 3.5 hours at 255 ℃ and 500r/min under nitrogen atmosphere, washing for 4 times by using deionized water, drying for 7.5 hours at 8Pa and 35 ℃ to obtain PTT fiber master batch, and mixing PTT fiber master batch, vinyl chitosan, azodiisobutyronitrile, camphene and methylene dichloride according to the mass ratio of 1:0.6:0.04:0.15:9, uniformly mixing, stirring for 9 hours at 25 ℃ and 500r/min to prepare a fiber spinning solution, loading the fiber spinning solution into a micro pump, adopting an ice plate covered with aluminum foil as a receiving device, adjusting the receiving distance to be 17cm, adjusting the voltage in the spinning process to be 24kV, adjusting the propulsion rate to be 0.65mL/h, adjusting the environmental temperature to be 25 ℃ and the spinning humidity to be 55%, and carrying out electrospinning in an electrostatic spinning device to prepare a primary PTT fiber, and drying the primary PTT fiber at 75 ℃ for 5.5 hours to prepare the bio-based PTT fiber.
Test example 1
Test of hygroscopicity
The testing method comprises the following steps: the examples and comparative examples were subjected to the moisture regain test according to GB/T6503-2017 method for testing chemical fibre moisture regain. The results are shown in Table 1.
TABLE 1
Moisture regain Moisture regain
Example 1 7.24% Comparative example 1 7.21%
Example 2 7.22% Comparative example 2 7.19%
Example 3 7.31% Comparative example 3 3.41%
Comparative example 4 7.42%
From the comparison of the experimental data of examples 1-3 and comparative examples 1-4 in Table 1, it can be found that the bio-based PTT fiber prepared by the present invention has good moisture absorption performance.
By comparison, the moisture regain of examples 1-3 is greater than that of comparative example 3, which shows that camphene is added as a pore-forming agent in the electrostatic spinning process to successfully form a porous structure on the bio-based PTT fiber, so that the specific surface area of the bio-based PTT fiber is improved, and meanwhile, the porous structure in the bio-based PTT fiber and the hydrophilic group on chitosan cooperate to endow the bio-based PTT fiber with excellent moisture absorption performance.
Test example 2
Testing of mechanical Properties
The testing method comprises the following steps: the mechanical properties of the examples and comparative examples were tested using an XL-1A filament reinforcement. The sample bypasses the yarn guide hook and the yarn guide wheel, passes through the upper clamp holder and the lower clamp holder downwards to ensure that the sample is straightened without looseness, applies about 10 cN of pre-tension to the sample, and returns to the original position after the lower clamp holder drives the sample to move downwards to the sample to fracture, so as to obtain the fracture strength of the sample. The clamping distance is 250 mm, the stretching speed is 250 mm/min, each sample is repeated for more than 10 times, and the test results are averaged. The results are shown in Table 2.
TABLE 2
Breaking strength (cN/dtex) Breaking strength (cN/dtex)
Example 1 4.47 Comparative example 1 1.79
Example 2 4.34 Comparative example 2 1.88
Comparative example 3 4.39 Comparative example 3 4.53
Comparative example 4 4.31
From the comparison of the experimental data of examples 1-3 and comparative examples 1-4 in Table 2, it can be found that the bio-based PTT fiber prepared by the invention has good mechanical properties.
By contrast, the breaking strength of examples 1-3 is greater than that of comparative example 1, which shows that vinyl chitosan is prepared by introducing double bonds on the molecular chains of chitosan through Schiff base reaction, and the double bonds on the vinyl chitosan are combined with P-H bonds on the main chain of the bio-based PTT fiber through phosphine addition to form a crosslinked structure, so that the relative slippage of the molecular chains in the bio-based PTT fiber is inhibited, and the mechanical properties of the bio-based PTT fiber are improved.
By contrast, the breaking strength of examples 1-3 is greater than that of comparative example 2, which shows that when PTT fiber oligomer is polymerized, dimethyl phosphite is added for copolymerization, P-H bonds are introduced on the molecular chain of the bio-based PTT fiber, and the P-H bonds are combined with double bonds on vinyl chitosan through phosphine addition to form a crosslinked structure, so that the relative sliding of the molecular chain in the bio-based PTT fiber is inhibited, and the mechanical property of the bio-based PTT fiber is improved.
Test example 3
Flame retardant Performance test
The testing method comprises the following steps: the limiting oxygen indices of the examples and comparative examples were tested in accordance with GB/T2406-93 using an oxygen index instrument. The results are shown in Table 3.
TABLE 3 Table 3
Limiting oxygen index Limiting oxygen index
Example 1 31.67% Comparative example 1 31.90%
Example 2 32.05% Comparative example 2 23.67%
Example 3 30.97% Comparative example 3 31.89%
Comparative example 4 32.12%
From the comparison of the experimental data of examples 1-3 and comparative examples 1-4 in Table 3, it can be found that the bio-based PTT fiber prepared by the invention has good flame retardant property.
By comparison, the limiting oxygen index of examples 1-3 is greater than that of comparative example 2, which shows that when PTT fiber oligomer is polymerized, dimethyl phosphite is added for copolymerization, and phosphorus element is introduced into the molecular chain of the bio-based PTT fiber, thereby improving the flame retardant property of the bio-based PTT fiber.
Test example 4
Washing resistance test
The testing method comprises the following steps: the examples and comparative examples were dried at 60℃for 3 hours, the weights were recorded, the effect of 50 times of household washing was simulated by using the BS5651-1978 method, the drying was performed at 60℃for 5 hours, the weights after washing were recorded, and the mass change rates before and after washing were calculated. The results are shown in Table 4.
TABLE 4 Table 4
Rate of mass change Rate of mass change
Example 1 1.56% Comparative example 1 1.90%
Example 2 1.67% Comparative example 2 1.67%
Example 3 1.12% Comparative example 3 1.44%
Comparative example 4 8.67%
From the comparison of the experimental data of examples 1-3 and comparative examples 1-4 in Table 4, it can be found that the bio-based PTT fiber prepared by the invention has good washing resistance.
By comparison, the mass change rate of examples 1-3 is smaller than that of comparative example 4, which shows that hydroxyl groups on the surface of the porous PTT fiber are converted into long carbon chains by transesterification, so that the washing resistance of the porous PTT fiber is improved.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (8)

1. The method for preparing the bio-based PTT fiber by recycling the waste fabric is characterized in that the method for preparing the bio-based PTT fiber by recycling the waste fabric is to prepare a PTT fiber master batch by reacting PTT fiber oligomer with dimethyl phosphite; mixing PTT fiber master batch with vinyl chitosan, a pore-forming agent and methylene dichloride, and preparing porous PTT fibers through electrostatic spinning; and then reacting the porous PTT fiber with methyl laurate.
2. The method for preparing the bio-based PTT fiber by recycling waste fabrics according to claim 1, wherein the PTT fiber oligomer is prepared by alcoholysis of the waste PTT fabrics with 1, 3-propanediol.
3. The method for preparing the bio-based PTT fiber by recycling waste fabrics according to claim 1, wherein the vinyl chitosan is prepared by reacting chitosan with acrolein.
4. The method for preparing the bio-based PTT fiber by recycling waste fabrics according to claim 1, wherein the pore-forming agent is camphene.
5. The method for preparing the bio-based PTT fiber by recycling waste fabrics according to claim 1, which is characterized by comprising the following preparation steps:
(1) Immersing waste PTT fabric into pure water for ultrasonic treatment for 2 hours, taking out, drying at 70-80 ℃ for 4-6 hours, crushing into PTT chips with the particle size smaller than 0.5mm by using a wall breaking machine, and mixing the PTT chips, 1, 3-propanediol and zinc acetate according to the mass ratio of 1:3: (0.01-0.03), stirring and refluxing for 1-2 hours at 200-210 ℃ and 600-800 r/min in a nitrogen atmosphere, cooling to 80-90 ℃, carrying out suction filtration with deionized water for 3-5 times to obtain filtrate, standing the filtrate at 0-2 ℃ for 24-36 hours, filtering, and drying at 70-80 ℃ for 5-6 hours to obtain PTT fiber oligomer;
(2) Chitosan, acetic acid and formaldehyde are mixed according to the mass ratio of 1: (2-3): (24-26) uniformly mixing, stirring at 20-30 ℃ for 1-2 hours at 300-500 r/min, adding acrolein with the mass 2-3 times of that of chitosan, stirring and refluxing at 50-60 ℃ for 8-10 hours at 300-500 r/min, drying at 5-10 Pa and 50-60 ℃ for 3-4 hours, washing with absolute ethyl alcohol for 3-5 times, and drying at 5-10 Pa and 50-60 ℃ for 4-6 hours to obtain vinyl chitosan;
(3) The PTT fiber oligomer, the dimethyl phosphite, the sodium hydroxide and the toluene are mixed according to the mass ratio of 1: (1-1.2): (0.03 to 0.05): (8-10) uniformly mixing, stirring and reacting for 3-4 hours at the temperature of 240-270 ℃ and the speed of 400-600 r/min under the nitrogen atmosphere, washing for 3-5 times by deionized water, drying for 7-8 hours at the temperature of 30-40 ℃ under the pressure of 5-10 Pa to obtain PTT fiber master batch, and mixing PTT fiber master batch, vinyl chitosan, azodiisobutyronitrile, camphene and methylene dichloride according to the mass ratio of 1: (0.5 to 0.7): (0.03 to 0.05): (0.1 to 0.2): (8-10) uniformly mixing, stirring for 8-10 hours at 20-30 ℃ at 400-600 r/min to prepare a fiber spinning solution, filling the fiber spinning solution into a micropump, adopting an ice plate covered with aluminum foil as a receiving device, adjusting the receiving distance to be 16-18 cm, controlling the voltage to be 23-25 kV in the spinning process, controlling the advancing rate to be 0.6-0.7 mL/h, controlling the environmental temperature to be 20-30 ℃ and the spinning humidity to be 50% -60%, and performing electrospinning in an electrospinning device to prepare a primary PTT fiber, and drying the primary PTT fiber at 70-80 ℃ for 5-6 hours to prepare the porous PTT fiber;
(4) The porous PTT fiber, methyl laurate and n-hexane are mixed according to the mass ratio of 1: (1-1.2): (8-10), uniformly mixing, stirring at 70-80 ℃ for reaction for 3-5 hours at 300-500 r/min, taking out, washing with absolute ethyl alcohol for 3-5 times, and drying at 70-80 ℃ for 4-6 hours to obtain the bio-based PTT fiber.
6. The method for preparing the bio-based PTT fiber by recycling waste fabrics according to claim 5, wherein the alcoholysis reaction process of the waste PTT fabrics in the step (1) is as follows:
。
7. the method for preparing the bio-based PTT fiber by recycling waste fabrics according to claim 5, wherein the reaction process of the vinyl chitosan in the step (2) is as follows:
。
8. the method for preparing the bio-based PTT fiber by recycling waste fabrics according to claim 5, wherein the reaction process of the porous PTT fiber in the step (3) is as follows:
。
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