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CN113136629A - Preparation process of high-strength and high-elongation para-aramid fiber - Google Patents

Preparation process of high-strength and high-elongation para-aramid fiber Download PDF

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Publication number
CN113136629A
CN113136629A CN202110397550.1A CN202110397550A CN113136629A CN 113136629 A CN113136629 A CN 113136629A CN 202110397550 A CN202110397550 A CN 202110397550A CN 113136629 A CN113136629 A CN 113136629A
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China
Prior art keywords
elongation
strength
aramid fiber
para
preparation process
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN202110397550.1A
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Chinese (zh)
Inventor
于安军
范志平
韩郡丰
武强强
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Zhongfang Special Fiber Co ltd
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Zhongfang Special Fiber Co ltd
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Priority to CN202110397550.1A priority Critical patent/CN113136629A/en
Publication of CN113136629A publication Critical patent/CN113136629A/en
Withdrawn legal-status Critical Current

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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/06Wet spinning methods
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00Treatment of filament-forming or like material
    • D01D1/06Feeding liquid to the spinning head
    • D01D1/09Control of pressure, temperature or feeding rate
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00Treatment of filament-forming or like material
    • D01D1/10Filtering or de-aerating the spinning solution or melt
    • D01D1/103De-aerating
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/06Washing or drying
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D4/00Spinnerette packs; Cleaning thereof
    • D01D4/02Spinnerettes
    • 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
    • D01F6/58Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/60Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
    • D01F6/605Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides from aromatic polyamides
    • 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
    • D01F6/78Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
    • D01F6/80Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyamides
    • D01F6/805Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyamides from aromatic copolyamides

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Artificial Filaments (AREA)

Abstract

The invention discloses a preparation method of para-aramid fiber with high strength and high elongation. The method comprises the steps of extruding an anisotropic spinning solution through capillary holes of a spinneret plate, spinning the anisotropic spinning solution through an air layer, entering a coagulating bath to obtain nascent fibers, and then washing and drying the nascent fibers. The method integrates the pore diameter of a spinneret plate, the temperature of a coagulation bath and tension control in the washing and drying processes, so that the high-strength and high-elongation fiber is obtained, the strength of the obtained fiber is more than 26g/d, and the elongation is more than 4.0%.

Description

Preparation process of high-strength and high-elongation para-aramid fiber
Technical Field
The invention belongs to the technical field of polymer synthesis, and particularly relates to a preparation process of para-aramid fiber with high strength and high elongation.
Background
Para-aramid fiber is initially developed and produced by DuPont company and is sold under the name of Kevlar, and is widely applied to the fields of aerospace, national defense and military industry, environmental protection, building and the like due to the characteristics of wear resistance, chemical corrosion resistance, high temperature resistance, high strength, high modulus, flame retardance and the like. For high-performance varieties, the method is always prohibited in China by being controlled as strategic materials by the West, and the research on aramid fibers in China since the 70 s has made a lot of remarkable progress, but the method has not made a complete technological breakthrough.
Patent US3869429 discloses a process for producing aramid fibers by an air layer spinning process, but there is no suggestion of the magnitude of the fiber washing tension, and although it is described that the fiber drying process can be carried out under a tension of less than 0.3g/d, its "zero tension" is shown only as a specific example of its low tension.
Patent US4016236 and patent US4560743 disclose a process for producing aramid fibers using a layer air spinning process where the fibers are carefully placed on a mesh belt for washing and drying to ensure that the fibers are not subjected to other tensions throughout the process.
Patent US4859393 discloses a method for preparing para-aramid fiber with high fatigue resistance by air layer spinning process, wherein the temperature of the coagulation bath is not lower than 20 ℃, the tension in the washing process is controlled to be 0.2 g/d-0.35 g/d, and the tension in the drying process is controlled to be 0.05 g/d-0.20 g/d.
Disclosure of Invention
The purpose of the invention is as follows: provides a preparation process of para-aramid fiber with high strength and high elongation.
The invention comprises the following steps: a preparation process of para-aramid fiber with high strength and high elongation comprises the following steps: step one, dissolving polymer resin in a sulfuric acid solution with a certain concentration to form an anisotropic spinning solution; extruding the spinning solution through capillary holes of a spinneret plate, and allowing the spinning solution to enter a low-temperature coagulating bath after passing through an air layer; and step three, washing and drying the obtained fiber under the condition of low tension.
The preferable technical scheme is as follows: the polymer resin is poly-p-phenylene terephthamide, which is a homopolymer obtained by polymerizing p-phenylene diamine and terephthaloyl chloride or a copolymer obtained by polymerizing a small amount of other diamine and p-phenylene diamine with a small amount of other diacid chloride and terephthaloyl chloride.
The preferable technical scheme is as follows: the concentration control range of the sulfuric acid is 90-100.5%, and the concentration control range of the anisotropic solution is 18.5-20%.
The preferable technical scheme is as follows: the acid concentration control range is 98-100.5%.
The preferable technical scheme is as follows: the aperture of the capillary hole of the spinneret plate is 0.0254 mm-0.0635 mm.
The preferable technical scheme is as follows: the pore diameter of the capillary hole of the spinneret plate is 0.0308 mm-0.0508 mm.
The preferable technical scheme is as follows: the control range of the temperature of the coagulating bath is-10 ℃ to 10 ℃.
The preferable technical scheme is as follows: the tension in the washing and drying processes is consistent, and the tension control range is 0.05 g/d-0.25 g/d.
The preferable technical scheme is as follows: the tension in the washing and drying processes is consistent, and the tension is 0.25 g/d.
The preferable technical scheme is as follows: the polymer resin has a melt viscosity of 6.0dL/g to 6.7 dL/g.
Compared with the prior art, the invention has the following beneficial effects: the strength of the prepared fiber is more than 26g/d, and the elongation is more than 4.0%.
Detailed Description
Example 1
Poly-p-phenylene terephthamide with the inherent viscosity of 6.3dL/g is dissolved in sulfuric acid with the concentration of 100.1 percent to form a spinning solution with the mass fraction of 19.4 percent, the solution passes through a spinneret plate with the pore diameter of a capillary hole of 0.0308mm after being degassed in vacuum, the temperature of the spinning solution is controlled to be 71 ℃, the height of an air layer is 0.64cm, the concentration of a coagulating bath is 8 percent, and the temperature of the coagulating bath is controlled to be 2 ℃. After the fiber comes out of the coagulating bath, the fiber sequentially passes through the steps of washing, neutralizing, drying, winding and the like, the tension in the washing and drying stages is measured before the fiber enters the working section, the tension is kept constant in the washing and drying processes, but the tension fluctuation of +/-10% is caused by the speed change of a rotating roller, and the fiber is dried on a hot steam roller with the surface temperature of 125 ℃. The strength of the prepared fiber is more than 27.3g/d, and the elongation is more than 4.5 percent.
Example 2 poly (p-phenylene terephthalamide) having an inherent viscosity of 6.3dL/g was dissolved in sulfuric acid having a concentration of 100.1% to form a spinning solution having a mass fraction of 19.4%, vacuum degassed, passed through a spinneret having a capillary hole diameter of 0.0508mm, the temperature of the spinning solution was controlled at 71 c, the height of the air layer was 0.64cm, the coagulation bath concentration was 8%, and the coagulation bath temperature was controlled at 2 c. After the fiber comes out of the coagulating bath, the fiber sequentially passes through the steps of washing, neutralizing, drying, winding and the like, the tension in the washing and drying stages is measured before the fiber enters the working section, the tension is kept constant in the washing and drying processes, but the tension fluctuation of +/-10% is caused by the speed change of a rotating roller, and the fiber is dried on a hot steam roller with the surface temperature of 125 ℃. The strength of the prepared fiber is more than 26.5g/d, and the elongation is more than 4.3 percent
Comparative examples a and B used spinneret capillary holes with a pore size of 0.0635mm and a tensile force during washing and drying of greater than 0.35g/d, resulting in fibers with a strength of less than 26g/d but an elongation of less than 4.0%.
Comparative example C used a spinneret capillary hole diameter of 0.0635mm, a coagulation bath temperature of greater than 10 ℃, and resulted in a fiber strength of less than 26 g/d. The comparative data are as follows:
Figure BDA0003019117700000031
Figure BDA0003019117700000041
the above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention are intended to fall within the protection scope defined by the claims of the present invention.

Claims (10)

1. A preparation process of para-aramid fiber with high strength and high elongation is characterized by comprising the following steps:
step one, dissolving polymer resin in a sulfuric acid solution with a certain concentration to form an anisotropic spinning solution;
extruding the spinning solution through capillary holes of a spinneret plate, and allowing the spinning solution to enter a low-temperature coagulating bath after passing through an air layer;
and step three, washing and drying the obtained fiber under the condition of low tension.
2. The process for preparing a high strength, high elongation para-aramid fiber as claimed in claim 1 wherein the polymer resin is poly (p-phenylene terephthalamide) which is a homopolymer obtained by polymerizing p-phenylene diamine and terephthaloyl chloride or a copolymer obtained by polymerizing a small amount of other diamines and p-phenylene diamine with a small amount of other diacid chlorides and terephthaloyl chloride.
3. The preparation process of the para-aramid fiber with high strength and high elongation as claimed in claim 1, wherein the concentration of the sulfuric acid is controlled within a range of 90-100.5%, and the concentration of the anisotropic solution is controlled within a range of 18.5-20%.
4. The preparation process of the para-aramid fiber with high strength and high elongation as claimed in claim 3, wherein the concentration of sulfuric acid is controlled within a range of 98-100.5%.
5. The process for preparing a high-strength high-elongation p-aramid fiber according to claim 1, wherein the pore size of the capillary hole of the spinneret is 0.0254mm to 0.0635 mm.
6. The process for preparing high-strength and high-elongation p-aramid fiber according to claim 5, wherein the pore size of the capillary hole of the spinneret plate is 0.0308mm to 0.0508 mm.
7. The preparation process of the para-aramid fiber with high strength and high elongation as claimed in claim 1, wherein the temperature control range of the coagulation bath is-10 ℃ to 10 ℃.
8. The preparation process of the para-aramid fiber with high strength and high elongation as claimed in claim 1, wherein the tension in the washing and drying processes is consistent, and the tension control range is 0.05 g/d-0.25 g/d.
9. The process for preparing a high-strength and high-elongation para-aramid fiber according to claim 8, wherein the tension during the washing and drying is uniform and is 0.25 g/d.
10. The process for preparing a high-strength high-elongation para-aramid fiber according to claim 1, wherein the polymer resin has a melt viscosity of 6.0dL/g to 6.7 dL/g.
CN202110397550.1A 2021-04-14 2021-04-14 Preparation process of high-strength and high-elongation para-aramid fiber Withdrawn CN113136629A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1710160A (en) * 2005-06-17 2005-12-21 东华大学 A method for preparing meta-aramid fibers
CN105926203A (en) * 2016-05-04 2016-09-07 江苏恒通印染集团有限公司 Oiling method for para-aramid fibers
CN106968021A (en) * 2017-04-06 2017-07-21 超美斯新材料股份有限公司 A kind of high-efficient spinning device
JP2018123457A (en) * 2017-02-02 2018-08-09 トヨタ紡織株式会社 Thermoplastic resin fiber, production method thereof, and fabric
CN112281223A (en) * 2019-07-26 2021-01-29 中蓝晨光化工有限公司 High-strength high-toughness para-aramid fiber and manufacturing method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1710160A (en) * 2005-06-17 2005-12-21 东华大学 A method for preparing meta-aramid fibers
CN105926203A (en) * 2016-05-04 2016-09-07 江苏恒通印染集团有限公司 Oiling method for para-aramid fibers
JP2018123457A (en) * 2017-02-02 2018-08-09 トヨタ紡織株式会社 Thermoplastic resin fiber, production method thereof, and fabric
CN106968021A (en) * 2017-04-06 2017-07-21 超美斯新材料股份有限公司 A kind of high-efficient spinning device
CN112281223A (en) * 2019-07-26 2021-01-29 中蓝晨光化工有限公司 High-strength high-toughness para-aramid fiber and manufacturing method thereof

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