CN110804767A - Aramid 1313 fiber and preparation method and application thereof - Google Patents

Aramid 1313 fiber and preparation method and application thereof Download PDF

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CN110804767A
CN110804767A CN201911067709.2A CN201911067709A CN110804767A CN 110804767 A CN110804767 A CN 110804767A CN 201911067709 A CN201911067709 A CN 201911067709A CN 110804767 A CN110804767 A CN 110804767A
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fiber
bath
aramid
stretching
preparation
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CN110804767B (en
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李永锋
刘键
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Ganzhou Longbang Material Technology Co Ltd
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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
    • D01F6/58Monocomponent 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G69/00Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
    • C08G69/02Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
    • C08G69/26Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
    • C08G69/32Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids from aromatic diamines and aromatic dicarboxylic acids with both amino and carboxylic groups aromatically bound
    • 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
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/12Stretch-spinning methods
    • D01D5/14Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Artificial Filaments (AREA)
  • Polyamides (AREA)

Abstract

The invention discloses an aramid 1313 fiber and a preparation method and application thereof, wherein the preparation method comprises the following steps: s1, one-bath forming: filtering the aramid polymer, defoaming in vacuum, storing at 20-90 ℃, filtering, and spraying in one-bath forming liquid to obtain nascent fiber; s2, forming in a second bath: spraying and molding the nascent fiber in the S1 by using a two-bath molding liquid to obtain a crude fiber; s3, three-bath stretching: stretching the crude fiber in the S2, washing with water, drying and sizing to obtain the fiber; wherein the one-bath forming liquid in S1 is a mixed solution of alcohols and amide solvents; the two-bath molding solution described in S2 is an amide solvent. The fiber strength of the invention reaches 6.0-9.0 cn/dtex, the elongation at break is 25-29%, the fiber strength is better, and the elongation at break reaches the national standard. The 1313 aramid fiber prepared by the method is high in strength and is suitable for preparing high-strength aramid materials.

Description

Aramid 1313 fiber and preparation method and application thereof
Technical Field
The invention relates to the field of aramid fiber preparation, and particularly relates to aramid 1313 fiber and a preparation method and application thereof.
Background
Aramid (Nomex is aramid fiber, and is phenylene terephthalamide), is a novel high-tech synthetic fiber, has excellent performances such as ultrahigh strength, high modulus, high temperature resistance, acid and alkali resistance, light weight, insulation, ageing resistance, long life cycle and the like, and is widely applied to the fields of composite materials, bulletproof products, building materials, special protective clothing, electronic equipment and the like. The aramid fiber 1313 is also called meta-aramid fiber, and is fully called m-phenylene isophthalamide, is one of aromatic polyamide fibers, has good flame retardance, thermal stability, electrical insulation, chemical stability, radiation resistance and mechanical properties, and is firstly developed and successfully realized by the U.S. DuPont company and industrialized production is realized. However, it is mostly applied in the fields of aerospace, automobile industry, special protective clothing, electrical insulation materials and the like, and is rarely applied in the national life field, particularly in the textile field.
The existing aramid fiber has the defects of poor interface adhesion and low interlaminar shear strength, and poor fiber strength generally, so that the interface bonding effect of the aramid fiber and a resin matrix needs to be improved. The patent CN2019105439484 discloses an aramid fiber ultrashort fiber and a preparation method thereof, the aramid fiber ultrashort fiber is prepared by mixing an aramid fiber polymer and a solidification solution in a specific proportion, the length of the prepared short fiber is 0.1-1 mm, the tearing strength is up to 2000-3000N, and the fiber still has the defect of poor bonding capability. Patent 2012103079088 provides a method for preparing black para-aramid fiber, in which carbon nanotubes are uniformly dispersed in aramid fiber, and the obtained aramid fiber has excellent linear density and strength, but has low elongation at break, even does not meet the national standard, and has complex preparation process, high cost and no contribution to industrial production.
Therefore, it is important to provide an aramid 1313 fiber having excellent fiber strength.
Disclosure of Invention
In view of the above problems in the prior art, the primary object of the present invention is to provide an aramid 1313 fiber.
The invention also aims to provide a preparation method of the aramid 1313 fiber.
Still another object of the present invention is to provide an application of the aramid 1313 fiber.
The technical scheme of the invention is as follows:
a preparation method of aramid 1313 fibers comprises the following steps:
s1, one-bath forming: filtering the aramid polymer through a filter medium, defoaming in vacuum to form a wiredrawing colloid, storing at 20-90 ℃, filtering for the second time, spraying, and spraying in a one-bath forming liquid to obtain nascent fiber;
s2, forming in a second bath: spraying and molding the nascent fiber in the S1 by using a two-bath molding liquid to obtain a crude fiber;
s3, three-bath stretching: stretching the crude fiber in the S2, washing with water, drying and sizing to obtain the fiber;
wherein the one-bath forming liquid in S1 is a mixed solution of alcohols and amide solvents; the two-bath molding solution described in S2 is an amide solvent.
The aramid polymer is prepared by the following method:
s11, adding a certain amount of amide solvent into a polymerization device filled with nitrogen;
s12, adding phenylenediamine into an amide polar organic solvent for dissolving, adding phthaloyl chloride, and carrying out polycondensation reaction at 0-20 ℃ to generate an aramid polycondensate and a byproduct hydrogen chloride;
s13, carrying out a neutralization reaction on the hydrogen chloride generated in the S12 by using alkaline earth metal oxides, hydroxides or ammonia gas and the like, wherein the reaction temperature is controlled to be lower than 30 ℃;
the concentration of the prepared aramid polymer is 10-22 wt%, [ η ] - [ 1.2-2.0, and the pH value is 6.8-7.3.
The spray head in the spinning in the S1 is a spherical spinning head, the aperture of the spherical spinning head is 0.05-0.3 mm, and the number of the holes is 5000-30000.
The stretching in the S3 process is three-stage stretching, the stretching multiple of each stage is 1-3 times, the total stretching multiple is 3-6 times, and the stretching temperature of each stage is room temperature.
Preferably, the one-bath forming liquid in S1 consists of the following substances in percentage by mass: 60-85% of alcohols, 5-30% of amide solvent and 0-10% of water.
More preferably, the one-bath forming liquid in S1 consists of the following substances in percentage by mass: 80% of alcohol and 20% of amide solvent.
Preferably, the temperature of the one-bath forming liquid in S1 is 20-50 ℃.
Preferably, the two-bath forming liquid in S2 is dimethylacetamide.
More preferably, the mass percentage concentration of the dimethylacetamide is 30-50%.
Preferably, the stretching liquid in S3 is a dimethylacetamide solution.
More preferably, the mass percentage concentration of the dimethylacetamide solution is 10-30%.
Preferably, the stretching in S3 is three-stage stretching, and the total stretching ratio is 4-6 times.
An aramid 1313 fiber prepared by any of the above methods is also within the scope of the invention.
An application of aramid 1313 fiber in preparing aramid material. The aramid 1313 fiber prepared by the preparation method provided by the invention has excellent fiber strength and bonding strength, and is very suitable for preparing aramid materials.
The beneficial technical effects of the invention are as follows:
the invention provides a preparation method of aramid 1313 fiber, the aramid 1313 fiber adopts aramid polymer as raw material, and the fiber is obtained by molding twice and drawing once, wherein the molding process of one-step molding is subjected to neutralization, filtration and defoaming treatment, the molding is carried out in one bath through a spray head to obtain nascent fiber, then the nascent fiber is stably molded again in two baths to obtain crude fiber, and finally the crude fiber is subjected to three-bath drawing, water washing, zone heating and drying and high-temperature vitrification temperature heat setting to obtain the aramid 1313 fiber. The strength of the conventional aramid 1313 fiber is 3.5-4.5 cn/dtex, while the strength of the fiber reaches 6.0-9.0 cn/dtex, the elongation at break is 25-29%, the fiber has better fiber strength, and the elongation at break reaches the national standard. The 1313 aramid fiber prepared by the method is high in strength and is completely suitable for preparing high-strength aramid materials.
Detailed Description
The present invention will be described in detail with reference to examples. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The aramid polymer is prepared by the following method:
s11, adding 7.5 parts of amide solvent into a polymerization device filled with nitrogen;
s12, adding 1.1 part of phenylenediamine into an amide polar organic solvent for dissolving, adding 1.86 parts of phthaloyl chloride, and carrying out polycondensation reaction at 0-20 ℃ to generate an aramid polycondensate and a byproduct hydrogen chloride;
s13, carrying out a neutralization reaction on the hydrogen chloride generated in the S12 by using alkaline earth metal oxides, hydroxides or ammonia gas and the like, wherein the reaction temperature is controlled to be lower than 30 ℃;
the prepared aramid polymer is light yellow and transparent, the concentration of the aramid polymer is 10-22 wt%, [ η ] - [ 1.2-2.0, and the pH value of the aramid polymer is 6.8-7.3.
Example 1
A preparation method of aramid 1313 fibers comprises the following steps:
s1, one-bath forming: filtering aramid polymer in a 30-micron filter press, defoaming in vacuum, filtering for the second time, and spraying out the aramid polymer in a one-bath forming bath through a spinneret with the number of 20000 holes and the diameter of 0.2mm to obtain nascent fiber;
s2, forming in a second bath: spraying and molding the nascent fiber in the S1 by using a two-bath molding liquid to obtain a crude fiber;
s3, three-bath stretching: stretching the crude fiber in S2, washing with water, drying at 110 ℃, and putting into a 330 ℃ crystallizer for crystallization and shaping to obtain the fiber;
wherein the one-bath forming liquid in the S1 comprises the following substances in percentage by mass: 80% of isobutanol and 20% of DMAC (dimethyl acetamide), and the temperature is 38 ℃;
the two-bath forming liquid in the S2 is dimethylacetamide with the mass percentage concentration of 43%;
the stretching liquid in S3 in which the total stretching ratio is 4.9 times the total stretching ratio is a dimethylacetamide solution having a mass percentage concentration of 20%.
Measuring the obtained aramid fiber according to GB/T14343-2008 to obtain the linear density of 2.9 Dtex;
the breaking strength was 8.0cn/dtex according to GB/T14337-2008 and the elongation at break was 26%.
Example 2
A preparation method of aramid 1313 fibers comprises the following steps:
s1, one-bath forming: filtering aramid polymer in a 20-micron filter press, defoaming in vacuum, filtering for the second time, and spraying out the aramid polymer in a one-bath forming bath through a spinneret with the number of holes being 18000 and the aperture being 0.08mm to obtain nascent fiber;
s2, forming in a second bath: spraying and molding the nascent fiber in the S1 by using a two-bath molding liquid to obtain a crude fiber;
s3, three-bath stretching: stretching the crude fiber in S2, washing with water, drying at 110 ℃, and putting into a 330 ℃ crystallizer for crystallization and shaping to obtain the fiber;
wherein the one-bath forming liquid in the S1 comprises the following substances in percentage by mass: 70% of isobutanol, 20% of DMAC, 10% of water and 20 ℃ of water;
the two-bath forming liquid in the S2 is dimethylacetamide with the mass percentage concentration of 30%;
the stretching liquid in S3 in which the total stretching ratio is 5.2 times the total stretching ratio is a dimethylacetamide solution having a mass percentage concentration of 20%.
Measuring the obtained aramid fiber according to GB/T14343-2008 to obtain the linear density of 2.7 Dtex;
the breaking strength was 7.1cn/dtex and the elongation at break was 26% as tested in GB/T14337-2008.
Example 3
A preparation method of aramid 1313 fibers comprises the following steps:
s1, one-bath forming: filtering aramid polymer in a 50-micron filter press, defoaming in vacuum, filtering for the second time, and spraying out the aramid polymer in a one-bath forming bath through a spinning nozzle with the number of holes of 5000 and the diameter of 0.05mm to obtain nascent fiber;
s2, forming in a second bath: spraying and molding the nascent fiber in the S1 by using a two-bath molding liquid to obtain a crude fiber;
s3, three-bath stretching: stretching the crude fiber in S2, washing with water, drying at 110 ℃, and putting into a 330 ℃ crystallizer for crystallization and shaping to obtain the fiber;
wherein the one-bath forming liquid in the S1 comprises the following substances in percentage by mass: 60% of isobutanol, 30% of DMAC, 10% of water and 50 ℃ of water;
the two-bath forming liquid in the S2 is dimethylacetamide with the mass percentage concentration of 50%;
the stretching liquid in S3 in which the total stretching ratio is 6.0 times the total stretching ratio is a dimethylacetamide solution having a mass percentage concentration of 20%.
Measuring the obtained aramid fiber according to GB/T14343-2008 to obtain the linear density of 2.8 Dtex;
the breaking strength was 6.1cn/dtex and the elongation at break was 29% as measured by GB/T14337-2008.
Comparative example 1
A preparation method of aramid 1313 fibers comprises the following steps:
s1, one-bath forming: filtering aramid polymer in a 30-micron filter press, defoaming in vacuum, filtering for the second time, and spraying out the aramid polymer in a one-bath forming bath through a spinneret with the number of 20000 holes and the diameter of 0.2mm to obtain nascent fiber;
s2, forming in a second bath: spraying and molding the nascent fiber in the S1 by using a two-bath molding liquid to obtain a crude fiber;
wherein the one-bath forming liquid in the S1 comprises the following substances in percentage by mass: 80% of isobutanol and 20% of DMAC (dimethyl acetamide), and the temperature is 38 ℃;
the two-bath forming liquid in the S2 is dimethylacetamide with the mass percentage concentration of 43%;
measuring the obtained aramid fiber according to GB/T14343-2008 to obtain the linear density of 1.9 Dtex;
the breaking strength was 5.0cn/dtex according to GB/T14337-2008, and the elongation at break was 14%.
Comparative example 2
A preparation method of aramid 1313 fibers comprises the following steps:
s1, one-bath forming: filtering aramid polymer in a 30-micron filter press, defoaming in vacuum, filtering for the second time, and spraying out the aramid polymer in a one-bath forming bath through a spinneret with the number of holes of 8000 and the diameter of 0.1mm to obtain nascent fiber;
s2, forming in a second bath: spraying and molding the nascent fiber in the S1 by using a two-bath molding liquid to obtain a crude fiber;
s3, three-bath stretching: stretching the crude fiber in S2, washing with water, drying at 120 ℃, and crystallizing and shaping in a crystallizer at 350 ℃ to obtain the fiber;
wherein the one-bath forming liquid in the S1 is dimethylacetamide with the mass percentage concentration of 50%; the others are water, and the temperature is room temperature;
the two-bath forming liquid in the S2 is dimethylacetamide with the mass percentage concentration of 53%;
the stretching in S3 was a stretching liquid having a total tertiary magnification of 3.1 times, and the stretching liquid was a dimethylacetamide solution having a mass percentage concentration of 20%.
Measuring the obtained aramid fiber according to GB/T14343-2008 to obtain the linear density of 2.1 Dtex;
the breaking strength was 4.1cn/dtex and the elongation at break was 18% as tested in GB/T14337-2008.
Comparative example 3
A preparation method of aramid 1313 fibers comprises the following steps:
s1, one-bath forming: spraying and molding the aramid polymer by using one-bath molding liquid to obtain crude fibers;
s2, stretching in a second bath: stretching the crude fiber in S1, washing with water, drying at 100 ℃, and putting into a crystallizer at 320 ℃ for crystallization and shaping to obtain the fiber;
wherein the one-bath forming liquid in the S1 is dimethylacetamide with the mass percentage concentration of 40%; the rest is water, and the temperature is room temperature;
the stretching in S2 is a stretching liquid having a total tertiary magnification of 4.2 times, and the stretching liquid is a dimethylacetamide solution having a mass percentage concentration of 25%.
Measuring the obtained aramid fiber according to GB/T14343-2008 to obtain the linear density of 2.0 Dtex;
the breaking strength was 3.8cn/dtex and the elongation at break was 30% as measured by GB/T14337-2008.
By comparing the examples and the comparative examples, the aramid 1313 fibers prepared in the examples have more excellent mechanical properties, wherein the linear density, the breaking strength and the breaking elongation are obviously better than those of the comparative examples.
While the embodiments of the present invention have been disclosed in the foregoing description, it is not limited to the applications listed in the description, but is capable of being applied in all kinds of fields adapted to the present invention, and it will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in the applications listed in the description without departing from the principle and spirit of the invention, and therefore the present invention is not limited to the details specified, without departing from the general concept defined by the claims and their equivalents.

Claims (10)

1. The preparation method of the aramid 1313 fiber is characterized by comprising the following steps of:
s1, one-bath forming: filtering the aramid polymer through a filter medium, defoaming in vacuum to form a wiredrawing colloid, storing at 20-90 ℃, filtering for the second time, spraying, and spraying in a one-bath forming liquid to obtain nascent fiber;
s2, forming in a second bath: spraying and molding the nascent fiber in the S1 by using a two-bath molding liquid to obtain a crude fiber;
s3, three-bath stretching: stretching the crude fiber in the S2, washing with water, drying and sizing to obtain the fiber;
wherein the one-bath forming liquid in S1 is a mixed solution of alcohols and amide solvents; the two-bath molding solution described in S2 is an amide solvent.
2. The method according to claim 1, wherein the one-bath forming liquid in S1 consists of, in mass percent: 60-85% of alcohols, 5-30% of amide solvent and 0-10% of water.
3. The method according to claim 2, wherein the one-bath forming liquid in S1 consists of, in mass percent: 80% of alcohol and 20% of amide solvent.
4. The method according to claim 1, wherein the temperature of the one-bath forming liquid in S1 is 20 to 50 ℃.
5. The method according to claim 1, wherein the two-bath forming liquid in S2 is dimethylacetamide.
6. The preparation method according to claim 5, wherein the mass percentage concentration of the dimethylacetamide is 30-50%.
7. The method according to claim 1, wherein the stretching liquid in S3 is a dimethylacetamide solution.
8. The method according to claim 1, wherein the stretching in S3 is a three-stage stretching, and the total stretching ratio is 4 to 6 times.
9. An aramid 1313 fiber prepared by the preparation method of any one of claims 1 to 8.
10. Use of the aramid 1313 fiber of claim 9 in the preparation of an aramid material.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114197076A (en) * 2020-09-18 2022-03-18 赣州龙邦材料科技有限公司 Preparation method of carbon nanotube aramid fiber and carbon nanotube aramid fiber
CN114197075A (en) * 2020-09-18 2022-03-18 赣州龙邦材料科技有限公司 Preparation method of carbon nanotube aramid fibrid and carbon nanotube aramid fibrid

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Publication number Priority date Publication date Assignee Title
US4842796A (en) * 1985-12-11 1989-06-27 Teijin Limited Process for producing high strength polymetaphenylene isophthalamide fiber
CN103526321A (en) * 2013-09-27 2014-01-22 东莞市灿森新材料有限公司 Preparation method of high-performance polyisophthaloyl metaphenylene diamine fiber
CN103668533A (en) * 2013-11-28 2014-03-26 圣欧芳纶(江苏)股份有限公司 Polyisophthaloyl metaphenylene diamine fiber and preparation method thereof
CN106757452A (en) * 2016-12-26 2017-05-31 中蓝晨光化工研究设计院有限公司 A kind of spinning process of aramid IIII fiber
CN109402761A (en) * 2018-10-24 2019-03-01 株洲时代新材料科技股份有限公司 A kind of preparation method of aramid fiber 1313 modified fibre

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4842796A (en) * 1985-12-11 1989-06-27 Teijin Limited Process for producing high strength polymetaphenylene isophthalamide fiber
CN103526321A (en) * 2013-09-27 2014-01-22 东莞市灿森新材料有限公司 Preparation method of high-performance polyisophthaloyl metaphenylene diamine fiber
CN103668533A (en) * 2013-11-28 2014-03-26 圣欧芳纶(江苏)股份有限公司 Polyisophthaloyl metaphenylene diamine fiber and preparation method thereof
CN106757452A (en) * 2016-12-26 2017-05-31 中蓝晨光化工研究设计院有限公司 A kind of spinning process of aramid IIII fiber
CN109402761A (en) * 2018-10-24 2019-03-01 株洲时代新材料科技股份有限公司 A kind of preparation method of aramid fiber 1313 modified fibre

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114197076A (en) * 2020-09-18 2022-03-18 赣州龙邦材料科技有限公司 Preparation method of carbon nanotube aramid fiber and carbon nanotube aramid fiber
CN114197075A (en) * 2020-09-18 2022-03-18 赣州龙邦材料科技有限公司 Preparation method of carbon nanotube aramid fibrid and carbon nanotube aramid fibrid

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