CN114672895A - Biomass composite fiber and its production method - Google Patents

Biomass composite fiber and its production method Download PDF

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Publication number
CN114672895A
CN114672895A CN202210329558.9A CN202210329558A CN114672895A CN 114672895 A CN114672895 A CN 114672895A CN 202210329558 A CN202210329558 A CN 202210329558A CN 114672895 A CN114672895 A CN 114672895A
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Prior art keywords
fiber
bacteriostatic agent
biocomposite
weight percentage
composite fiber
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CN202210329558.9A
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Inventor
何建桦
刘国雄
汤敦仁
朱永伟
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent 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
    • D01F6/92Monocomponent 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
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/103Agents inhibiting growth of microorganisms
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent

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  • 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 a biodegradable biomass composite fiber, comprising: at least one biomass and at least one organic compatibilizer. The at least one biomass material includes, for example, at least one of polybutylene succinate, polylactic acid, polybutylene terephthalate adipate; the at least one organic compatibilizer includes at least one of glycerin, montan wax, polyvinyl alcohol, butyl citrate triester, and epoxidized soybean oil. The present invention also provides a method for preparing the biomass composite fiber, wherein the biomass composite fiber prepared by the pre-oriented yarn or melt-blown spinning process can be applied to various textiles to replace synthetic fibers prepared from petrochemical products.

Description

Biomass composite fiber and its production method
Technical Field
The present invention relates to composite fiber, and is especially one kind of microbial degradable biomass composite fiber and its preparation process.
Background
Since the synthetic chemical fibers produced by petrochemicals are rich in the aspects of textiles and articles in daily life, the chemical fibers have serious impact and ecological damage on environmental pollution, and how to improve the situation to enable the human environment to develop forever is one of the most important issues.
Polylactic acid (PLA) is used in textile by spinning in the early century, and has attracted global attention, and this biomass (Bio-mass) material can replace a large amount of chemical fiber products produced by the traditional petrochemical industry, such as: five plastics, polyester blend … and the like.
Recently, the formulation and manufacturing process of spinning raw biomass materials have been improved with the environmental awareness of the public, and have been paid attention to and developed new products, and the trend of saving energy and reducing carbon is only reflected by the common use of organic solvent hot melt spinning filament, high temperature melt spinning short filament or continuous filament.
Therefore, it is necessary to provide a multifunctional green biomass composite fiber with low melting point and no solvent and a method for preparing the same, so as to solve the above problems.
Disclosure of Invention
The main object of the present invention is to provide a biomass composite fiber which is completely biodegradable, and a method for producing the same.
To achieve the above object, the present invention provides a biomass composite fiber comprising: at least one biopolymer and at least one organic compatibilizer. The at least one biopolymer includes at least one of Polybutylene succinate (Bio-Polybutylene succinate, Bio-PBS), Polylactic acid (PLA), and Polybutylene terephthalate (PBAT). The at least one organic compatibilizer includes at least one of Glycerol (Glycerol), Montan wax (Montan wax), Polyvinyl alcohol (PVA), butyl citrate Triester (TBC), and Epoxidized Soybean Oil (ESO). Wherein, in the biocomposite fiber, the weight percentage of the at least one biocomposite polymer is not less than 80 wt.%, and the weight percentage of the at least one organic compatibilizer is between 1 wt.% and 10 wt.%.
Preferably, the biomass composite fiber further comprises a plurality of filler particles, wherein the weight percentage of the plurality of filler particles in the biomass composite fiber is between 0.5 wt.% and 5 wt.%.
Preferably, the antibacterial agent is further included, wherein the weight percentage of the antibacterial agent in the biomass composite fiber is between 1 wt.% and 10 wt.%.
Preferably, the bacteriostatic agent comprises at least one of distilled wood vinegar, distilled bamboo vinegar, wood vinegar powder and bitter tea seed powder.
Preferably, the bacteriostatic agent further comprises at least one of glycerol, Triton X-100 and tributyl citrate.
Preferably, a plurality of filler particles are further included, wherein in the biocomposite fiber, the weight percentage of the at least one biopolymer is between 90 wt.% and 97 wt.%, the weight percentage of the at least one organic compatibilizer is between 1.5 wt.% and 7 wt.%, the weight percentage of the plurality of filler particles is between 0.5 wt.% and 2.5 wt.%, and the weight percentage of the bacteriostatic agent is between 1 wt.% and 6 wt.%; the plurality of filler particles comprises at least one of nano calcium carbonate and calcium oxide; and the bacteriostatic agent comprises wood vinegar.
In order to achieve the above object, the present invention further provides a method for producing a biomass composite fiber, comprising the steps of: preparing a premix comprising not less than 80 wt.% of at least one biopolymer and 1 wt.% to 10 wt.% of at least one organic compatibilizer; heating and melting the premix to form a melt; and spinning the melt to form a biocomposite fiber. Wherein the at least one biopolymer comprises a material selected from at least one of polybutylene succinate, polylactic acid, and polybutylene terephthalate-adipate; the at least one organic compatibilizer comprises a material selected from at least one of glycerin, montan wax, polyvinyl alcohol, butyl citrate triester, and epoxidized soybean oil.
Preferably, the melt has a melt index of between 30gm/10min and 55gm/10min at 190 ℃.
Preferably, the premix is formed by mixing the at least one biopolymer and the at least one organic compatibilizer, and optionally adding a bacteriostatic agent and at least one of a plurality of filler particles; the bacteriostatic agent comprises an active ingredient selected from at least one of distilled wood vinegar, distilled bamboo vinegar, wood vinegar powder, and bitter tea seed powder; and the plurality of filler particles are selected from at least one of nano calcium carbonate and calcium oxide.
Preferably, not less than 60 wt.% of the active ingredient is mixed with an auxiliary agent and heated at a heating temperature of 62 ℃ to 74 ℃ for at least 3 hours to form the bacteriostatic agent, wherein the auxiliary agent is at least one selected from glycerol, Triton X-100 and tributyl citrate.
The invention has the advantages that:
the biomass composite fiber provided by the invention is completely biodegradable.
Drawings
Is composed of
Detailed Description
The following description is given by way of example only, and is not intended to limit the scope of the invention.
The biomass composite fiber comprises at least one biomass polymer and at least one organic mutual compatilizer. The at least one biopolymer includes at least one of Polybutylene succinate (Bio-Polybutylene succinate, Bio-PBS), Polylactic acid (PLA), and Polybutylene terephthalate (PBAT). The at least one organic compatibilizer includes at least one of Glycerol (Glycerol), Montan wax (Montan wax), Polyvinyl alcohol (PVA), butyl citrate Triester (TBC), and Epoxidized Soybean Oil (ESO). Wherein, in the biocomposite fiber, the weight percentage of the at least one biocomposite polymer is not less than 80 wt.%, and the weight percentage of the at least one organic compatibilizer is between 1 wt.% and 10 wt.%. Therefore, the biomass composite fiber can be applied to various textiles, such as but not limited to clothes, diapers, sanitary napkins, bed sheets, quilt covers, wet tissues … and the like, can be decomposed and dissolved into soil under general environment, completely belongs to a high-quality new material with environment friendliness and no toxicity, meets the requirements of current green environmental protection, and is beneficial to maintaining natural ecology and the world trend of sustainable development.
Preferably, the biocomposite fiber further comprises a plurality of filler particles, such as but not limited to powder, particles, irregular particles …, etc., the weight percentage of the plurality of filler particles in the biocomposite fiber is between 0.5 wt.% and 5 wt.%; the plurality of filler particles include at least one of nanocalcium carbonate and calcium oxide, are lightweight, and increase the strength of the biocomposite fiber.
Preferably, the biomass composite fiber further comprises a bacteriostatic agent, and the weight percentage of the bacteriostatic agent in the biomass composite fiber is between 1 wt.% and 10 wt.%, so that the bacteriostatic agent provides insect-proof and deodorant effects. The bacteriostatic agent comprises at least one of Distilled pyroligneous acid, Distilled bamboo Vinegar, Vinegar powder and bitter tea seed powder as an active ingredient, wherein the active ingredient is natural and is environment-friendly after decomposition. The bacteriostatic agent further comprises at least one of glycerol, Triton X-100 and tributyl citrate as an auxiliary agent, so that the bacteriostatic agent and the at least one biomass material have better compatibility and can be uniformly distributed. The auxiliary agent may also include, for example but not limited to, surfactants such as Tween series, Span series …, and the like, and may be combined and selected according to the material requirements.
In detail, in the biomass composite fiber, the weight percentage of the at least one biomass polymer is between 90 wt.% and 97 wt.%, the weight percentage of the at least one organic compatibilizer is between 1.5 wt.% and 7 wt.%, the weight percentage of the plurality of filler particles is between 0.5 wt.% and 2.5 wt.%, and the weight percentage of the bacteriostatic agent is between 1 wt.% and 6 wt.%, so that the biomass composite fiber is entirely biodegradable material, is environmentally friendly and strong, and also has insect-proof and deodorizing effects.
The invention also provides a method for preparing the biomass composite fiber, which is used for preparing the biomass composite fiber and comprises the following steps:
preparing a premix comprising not less than 80 wt.% of the at least one biopolymer and 1 wt.% to 10 wt.% of the at least one organic compatibilizer. Further, the premix is formed by mixing the at least one biopolymer and the at least one organic compatibilizer, and optionally adding the bacteriostatic agent and at least one of the plurality of filler particles; mixing not less than 60 wt.% of the active ingredient with an auxiliary agent, and heating at a heating temperature of 62-74 ℃ for at least 3 hours to form the bacteriostatic agent, thereby improving the compatibility of the bacteriostatic agent with the at least one biopolymer and avoiding the damage of the active ingredients.
The premix is heated to melt the premix to form a melt. Preferably, the Melt has a Melt Index (MI) of 30-55 gm/10min (2.16kg load) at 190 ℃ to have proper fluidity for subsequent formation of filaments, staple fibers, etc. without breaking.
Spinning the melt to form the biocomposite fiber. The Melt may be formed into the biocomposite fiber, for example, by spinning processes such as drawing, Pre-Oriented Yarn (POY), Melt blowing (Melt blow), and the like. In addition, the melt can be formed into initial pellets by a pelletizer so as to be convenient for storage, transportation and the like, and subsequent spinning can be carried out without difficulty.
The invention is further illustrated by the following examples.
Example 1:
97 wt.% of polybutylene terephthalate adipate raw material particles, 2.5 wt.% of polyvinyl alcohol and 0.5 wt.% of epoxidized soybean oil which are dried to be less than 100ppm of moisture are weighed, the raw material particles, the polyvinyl alcohol and the epoxidized soybean oil are put into a stirrer together to be fully and uniformly mixed into a premix, the premix is poured into a feeding funnel of a spinning extruder, and the spinning extruder is started to start heating.
When a heating section of the spinning extruder reaches a set temperature, starting a screw of the spinning extruder to extrude the molten premix through two spinneret plates with 72 holes in total so as to extrude a plurality of continuous filaments, solidifying the filaments through an air cooling channel, pinching and pressing the filaments into a single filament bundle by a twisting oil seat, and forming the biomass composite fiber, wherein the biomass composite fiber is wound on a winding wheel set and then wound on a yarn drum; wherein the spinning speed is regulated to be about 340 m/min. Therefore, the biomass composite fiber can be spun by a pre-oriented yarn method, and is a yarn roll of bright silver white filaments with the fineness of about 13.2dpf (denier per fiber).
Example 2:
weighing 80 wt% of dried poly (adipic acid-p-xylylene glycol) butanediol ester, 12 wt% of polylactic acid, 4 wt% of polyvinyl alcohol, 0.5 wt% of montan wax, 1.5 wt% of soybean epoxy oil and 2 wt% of nano calcium carbonate, and sequentially putting the materials into a high-speed stirrer to be uniformly mixed to form the premix.
The premix was poured into a feed hopper of a twin screw granulator and heating was started. When a heating section of the twin-screw granulator reaches a set temperature, the premix is subjected to bracing, cooling and cutting in sequence to produce a plurality of initial granules. Wherein the premix has a melt index of about 39.2gm/10min at 190 ℃ under a load of 2.16 kg.
Placing the plurality of initial material particles into a feeding hopper of a spinning machine, extruding continuous plurality of filaments from the molten premix when a heating section of the spinning machine reaches a set temperature, solidifying the plurality of filaments to form the biomass composite fiber, and winding the plurality of filaments on a yarn barrel through a winding wheel; wherein the spinning speed is regulated to be about 300m/min to 400 m/min. The biomass composite fiber is a white yarn roll, and the fineness of the yarn roll is about 10 dpf.
Example 3:
taking 75 wt.% of rectified pyroligneous liquor by a measuring cylinder, taking 25 wt.% of anhydrous glycerol by another measuring cylinder, putting the rectified pyroligneous liquor and the anhydrous glycerol into a 1L beaker together, heating and stirring to form a mixture, controlling the mixture to be steamed and boiled at 62-68 ℃ for 4 hours until the weight of the mixture is reduced to about 80 wt.% of the original weight, stopping stirring and heating, and cooling to obtain the natural biological bacteriostatic agent.
Weighing 75 wt% of dried poly (adipic acid-p-xylylene glycol) terephthalate, 15 wt% of polylactic acid, 4.5 wt% of polyvinyl alcohol, 0.5 wt% of montan wax, 1.8 wt% of epoxidized soybean oil, 1.2 wt% of nano calcium carbonate and 2 wt% of the bacteriostatic agent, and sequentially putting the materials into a high-speed stirrer to be uniformly mixed to form the premix.
Pouring the premix into a feeding hopper of a twin-screw granulator, and when a heating section of the twin-screw granulator reaches a set temperature, sequentially carrying out bracing, cooling and cutting on the premix to produce a plurality of initial granules. Wherein the premix has an average of about 49gm/10min for four melt indices at 190 ℃ under a load of 2.16 kg.
Placing the plurality of initial material particles into a feeding hopper of a spinning machine, extruding the molten premix through a spinneret plate to extrude a plurality of continuous, fine and vertical filaments when a heating section of the spinning machine reaches a set temperature, bundling the plurality of filaments into a single filament bundle by a filament twisting oil seat to form the biomass composite fiber, and spinning the biomass composite fiber around three to four pairs of winding wheel sets with fixed rotating speed and then winding the biomass composite fiber on a yarn barrel; wherein the biomass composite fiber is a yarn roll with fineness of about 5.5dpf, light honey brown color and wood vinegar flavor.
Example 4:
weighing 60 wt% of rectified pyroligneous liquor, 1.5 wt% of surfactant and 38.5 wt% of tributyl citrate, putting the components into a 1L beaker together, starting heating and stirring to form a mixture, controlling the mixture to be steamed and boiled at 69-74 ℃ for 4 hours until the weight of the mixture is reduced to about 50 wt% of the original weight, stopping stirring and heating, and cooling to obtain the natural biological bacteriostatic agent.
Weighing 30 wt% of dried polybutylene succinate, 40 wt% of dried polybutylene adipate-terephthalate, 22 wt% of polylactic acid, 3 wt% of polyvinyl alcohol and 5 wt% of the bacteriostatic agent, and sequentially putting the materials into a high-speed stirrer to be uniformly mixed to form the premix.
Pouring the premix into a feeding hopper of a twin-screw granulator, and when a heating section of the twin-screw granulator reaches a set temperature, sequentially carrying out bracing, cooling and cutting on the premix to produce a plurality of initial granules. Wherein the premix has an average of four melt indices of about 47.3gm/10min at 190 ℃ under a load of 2.16 kg.
The plurality of initial material particles are put into a feeding hopper of a melt-blowing machine, when a heating section of the melt-blowing machine reaches a set temperature, a screw rod is rotated to adjust the air injection pressure of the melt-blowing machine so as to enable the plurality of molten initial material particles to extrude through a T-shaped melt-blowing die head, short silk flow which is blown off and sprayed is attached to a negative suction conveying belt with a certain speed, and then the short silk flow is wound into non-woven fabric cakes through a rolling roller set.

Claims (10)

1. A biocomposite fiber, comprising:
at least one biopolymer including at least one of polybutylene succinate, polylactic acid, and polybutylene terephthalate-adipate; and
at least one organic compatibilizer comprising at least one of glycerin, montan wax, polyvinyl alcohol, butyl citrate triester, and epoxidized soybean oil;
wherein, in the biocomposite fiber, the weight percentage of the at least one biocomposite polymer is not less than 80 wt.%, and the weight percentage of the at least one organic compatibilizer is between 1 wt.% and 10 wt.%.
2. The biocomposite fiber of claim 1, further comprising a plurality of filler particles, wherein the weight percentage of the plurality of filler particles in the biocomposite fiber is between 0.5 wt.% and 5 wt.%.
3. The biocomposite fiber of claim 1, further comprising a bacteriostatic agent, wherein the bacteriostatic agent is present in the biocomposite fiber in an amount of 1 wt.% to 10 wt.%.
4. The biomass composite fiber according to claim 3, wherein the bacteriostatic agent comprises at least one of distilled wood vinegar, distilled bamboo vinegar, wood vinegar powder, and bitter tea seed powder.
5. The biocomposite fiber of claim 4, wherein the bacteriostatic agent further comprises at least one of glycerol, Triton X-100, and tributyl citrate.
6. The biocomposite fiber of claim 4, further comprising a plurality of filler particles, wherein in the biocomposite fiber, the weight percentage of the at least one biopolymer is between 90 wt.% and 97 wt.%, the weight percentage of the at least one organic compatibilizer is between 1.5 wt.% and 7 wt.%, the weight percentage of the plurality of filler particles is between 0.5 wt.% and 2.5 wt.%, and the weight percentage of the bacteriostatic agent is between 1 wt.% and 6 wt.%; the plurality of filler particles comprises at least one of nano calcium carbonate and calcium oxide; and the bacteriostatic agent comprises wood vinegar.
7. The method for preparing the biomass composite fiber is characterized by comprising the following steps of:
preparing a premix comprising not less than 80 wt.% of at least one biopolymer and 1 wt.% to 10 wt.% of at least one organic compatibilizer;
heating and melting the premix to form a melt; and
spinning the melt to form a biomass composite fiber;
wherein the at least one biopolymer comprises a material selected from at least one of polybutylene succinate, polylactic acid, and polybutylene terephthalate-adipate; the at least one organic compatibilizer comprises a material selected from at least one of glycerin, montan wax, polyvinyl alcohol, butyl citrate triester, and epoxidized soybean oil.
8. The method of claim 7, wherein the melt index at 190 ℃ is controlled to be between 30gm/10min and 55gm/10 min.
9. The method of claim 7, wherein the premix is formed by mixing the at least one biopolymer and the at least one organic compatibilizer, and optionally adding a bacteriostatic agent and at least one of a plurality of filler particles; the bacteriostatic agent comprises an active ingredient selected from at least one of distilled wood vinegar, distilled bamboo vinegar, wood vinegar powder, and bitter tea seed powder; and the plurality of filler particles are selected from at least one of nano calcium carbonate and calcium oxide.
10. The method of claim 9, further comprising mixing not less than 60 wt.% of the active ingredient with an auxiliary agent and heating the mixture at a temperature of 62 ℃ to 74 ℃ for at least 3 hours to form the bacteriostatic agent, wherein the auxiliary agent is at least one selected from the group consisting of glycerin, Triton X-100, and tributyl citrate.
CN202210329558.9A 2022-03-31 2022-03-31 Biomass composite fiber and its production method Pending CN114672895A (en)

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JPH0598264A (en) * 1991-10-09 1993-04-20 Sanin Netsukaritsuchi:Kk Wood vinegar powder and preparation thereof
JPH10102323A (en) * 1996-09-27 1998-04-21 Toray Monofilament Co Ltd Biodegradable conjugate monofilament and its use
TW442592B (en) * 2000-03-30 2001-06-23 Yuen Foong Yu Paper Mfg Co Ltd Multifunctional paper and method for making the same
JP2004215550A (en) * 2003-01-14 2004-08-05 Toshiyuki Aeba Fibrous product for raising seedling and method for producing the same
TW200801113A (en) * 2006-06-27 2008-01-01 Far Eastern Textile Ltd The polylactic acid composition and the deep dyeing fiber manufactured from the same
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Application publication date: 20220628