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 PDFInfo
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- 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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- Prior art keywords
- elongation
- strength
- aramid fiber
- para
- preparation process
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- 239000000835 fiber Substances 0.000 title claims abstract description 39
- 229920003235 aromatic polyamide Polymers 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 18
- 238000009987 spinning Methods 0.000 claims abstract description 16
- 230000001112 coagulating effect Effects 0.000 claims abstract description 8
- 230000015271 coagulation Effects 0.000 claims abstract description 6
- 238000005345 coagulation Methods 0.000 claims abstract description 6
- 239000011148 porous material Substances 0.000 claims abstract description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 239000002952 polymeric resin Substances 0.000 claims description 6
- 229920003002 synthetic resin Polymers 0.000 claims description 6
- 229920006231 aramid fiber Polymers 0.000 claims description 5
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 4
- 230000000379 polymerizing effect Effects 0.000 claims description 4
- LXEJRKJRKIFVNY-UHFFFAOYSA-N terephthaloyl chloride Chemical compound ClC(=O)C1=CC=C(C(Cl)=O)C=C1 LXEJRKJRKIFVNY-UHFFFAOYSA-N 0.000 claims description 4
- 229920001577 copolymer Polymers 0.000 claims description 2
- 150000004985 diamines Chemical class 0.000 claims description 2
- 229920001519 homopolymer Polymers 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims description 2
- 229920003366 poly(p-phenylene terephthalamide) Polymers 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- 150000001805 chlorine compounds Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 239000004760 aramid Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 125000001140 1,4-phenylene group Chemical group [H]C1=C([H])C([*:2])=C([H])C([H])=C1[*:1] 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229920000271 Kevlar® Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000004761 kevlar Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/06—Feeding liquid to the spinning head
- D01D1/09—Control of pressure, temperature or feeding rate
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/10—Filtering or de-aerating the spinning solution or melt
- D01D1/103—De-aerating
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/06—Washing or drying
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D4/00—Spinnerette packs; Cleaning thereof
- D01D4/02—Spinnerettes
-
- 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
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
- D01F6/605—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides from aromatic polyamides
-
- 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
- D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
- D01F6/80—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyamides
- D01F6/805—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyamides from aromatic copolyamides
Landscapes
- 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
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:
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.
Priority Applications (1)
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CN202110397550.1A CN113136629A (en) | 2021-04-14 | 2021-04-14 | Preparation process of high-strength and high-elongation para-aramid fiber |
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CN202110397550.1A CN113136629A (en) | 2021-04-14 | 2021-04-14 | Preparation process of high-strength and high-elongation para-aramid fiber |
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Citations (5)
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 |
-
2021
- 2021-04-14 CN CN202110397550.1A patent/CN113136629A/en not_active Withdrawn
Patent Citations (5)
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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Application publication date: 20210720 |
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