CN117306013A - Preparation method of paper-making-grade meta-aramid fiber surface brooming - Google Patents

Preparation method of paper-making-grade meta-aramid fiber surface brooming Download PDF

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Publication number
CN117306013A
CN117306013A CN202311278861.1A CN202311278861A CN117306013A CN 117306013 A CN117306013 A CN 117306013A CN 202311278861 A CN202311278861 A CN 202311278861A CN 117306013 A CN117306013 A CN 117306013A
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Prior art keywords
meta
aramid
fiber
temperature
dimethylacetamide
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Inventor
蒋少波
李永锋
李健灿
黄振宇
蒋泉洪
董晓亮
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Ganzhou Longbang Material Technology Co ltd
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Ganzhou Longbang Material Technology Co ltd
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Priority to CN202311278861.1A priority Critical patent/CN117306013A/en
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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
    • D01F6/90Monocomponent 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 polyamides
    • D01F6/905Monocomponent 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 polyamides of aromatic polyamides
    • 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
    • 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
    • D01F1/04Pigments
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/62Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Paper (AREA)

Abstract

The invention belongs to the technical field of meta-aramid fiber surface treatment, and discloses a preparation method of the surface fibrillation of paper-making grade meta-aramid fiber, which comprises the steps of synthesizing, neutralizing, spinning and chopping colored 1313 meta-aramid polymer, conveying the meta-aramid polymer into a spinneret through a metering pump, spraying the meta-aramid polymer into a coagulating bath forming liquid to form primary fibers, forming bubbles by the gasification phenomenon of organic solvents dimethyl acetamide and water which are uniformly distributed in the primary fibers due to the great improvement of the coagulating temperature, and cracking the surface with less pressure from the inside to the periphery of the fibers, taking out the fiber as a fibrillated fiber, prolonging the forming time of the fiber in the coagulating bath to 1-5min, obtaining better coagulating effect, keeping the strength of the meta-aramid fiber of a paper-making grade finished product to be more than 3.8cn/dtex, simultaneously having more excellent cohesive force, intertwining the fibers with each other when making paper, improving the bonding point and bonding strength, and realizing high-performance paper strength and tearing strength.

Description

Preparation method of paper-making-grade meta-aramid fiber surface brooming
Technical Field
The invention belongs to the technical field of meta-aramid fiber surface treatment, and particularly relates to a preparation method for surface fibrillation of paper-grade meta-aramid fiber.
Background
The aramid fiber is a novel high-tech synthetic fiber, has excellent performances of ultrahigh strength, high modulus, high temperature resistance, acid and alkali resistance, light weight, insulation, aging 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 1313 is also called meta-aramid, is called m-phenylene isophthalamide, is an aromatic polyamide fiber, has good flame retardance, heat stability, electrical insulation, chemical stability, radiation resistance and mechanical property, and is developed and successfully achieved by DuPont company in U.S. for the earliest time and achieves industrial production. But it is mostly applied in the fields of aerospace, automobile industry, special protective clothing, electric insulation materials and the like.
At present, meta-aramid is mostly converted into aramid paper through a papermaking process and equipment, and then the aramid paper is applied to the fields of insulation, honeycomb and circuit boards, so that the quality of the prepared aramid paper is particularly critical, and one excellent meta-aramid paper needs high-performance tensile strength, tearing degree and dielectric strength.
In the paper making process of the plant fiber, the plant fiber is subjected to fibrillation treatment by a beater, so that the fiber cell wall is fluffed, torn, split and the like, and the fibrillation is realized by the mechanical action of the beater, so that the two ends of the plant fiber are split to be similar to a broom. The plant pulp fiber is greatly improved in cohesion through the fibrillation, the binding points and the binding strength are improved when the plant pulp fiber is entangled with each other during paper making, and finally the aim of improving the tensile strength and the tearing strength of paper is achieved. The aim of improving the tensile strength and the tearing strength by the surface fibrillation or the roughness increase of the meta-aramid chopped fiber cannot be achieved.
In the prior art, meta-aramid paper is prepared from meta-aramid chopped fibers and meta-aramid fibrids through a papermaking and hot rolling process, wherein the meta-aramid chopped fibers play a role in improving the stiffness, tensile strength and tear strength of paper in the aramid paper; meta-aramid fibrid plays roles of adhesion and tensile strength improvement in aramid paper; the meta-aramid chopped fiber is a novel high-tech chemical synthetic fiber, the fiber surface is very smooth, the cross section is mainly round, so that the cohesion force of the meta-aramid chopped fiber to the meta-aramid chopped fiber is not enough, the tensile strength and the tearing degree are low, the meta-aramid chopped fiber is easy to tear and break due to the pulling action in the application field of the rear end of the aramid paper, the yield is reduced, the cross section of the meta-aramid fiber is improved in the market at present, for example, the cross section is changed into a polygon, a star shape, an irregular kidney bean shape or an ellipse shape, and the like, the transverse area of the fiber is enlarged, the cohesion force of the meta-aramid chopped fiber to the meta-aramid chopped fiber in the secondary direction is increased, the effect is not obvious although the meta-aramid chopped fiber is improved, the fiber surface is still smooth, and the longitudinal state still has no force point.
Disclosure of Invention
The invention aims to provide a preparation method for surface fibrillation of a paper-making-grade meta-aramid fiber, which aims to solve the problems of uneven coloring, low coloring efficiency, low color fastness of post-dyeing and limited application field of the existing colored fiber of meta-aramid fiber before spinning.
In order to achieve the above object, the present invention provides the following technical solutions: the preparation method of the paper-making grade meta-aramid fiber surface brooming comprises the steps of synthesis, neutralization, spinning and chopping of colored 1313 meta-aramid polymer, wherein the synthesis of the colored 1313 meta-aramid polymer comprises the following steps:
sp1: m-phenylenediamine is dissolved in amide polar organic solvent DMAC;
sp2: controlling the reaction temperature to be-10 ℃ to 0 ℃, and adding the corresponding amount of 90wt% to 95wt% of isophthaloyl dichloride to carry out low-temperature polycondensation reaction;
sp3: adding a colored pigment, and adding 5-10wt% of isophthaloyl dichloride with the residual corresponding amount to continue the low-temperature polycondensation reaction;
sp4: the byproduct hydrogen chloride is subjected to a neutralization reaction by adopting alkaline earth metal oxide, hydroxide or ammonia gas, and the temperature of the neutralization reaction is controlled to be lower than 30 ℃; the concentration of the obtained meta-aramid polymer is 15-25 wt%, eta is 1.7-2.5, and the pH value is 4-7;
the spinning of the colored 1313 meta-aramid polymer comprises the following steps:
sp5: filtering meta-aramid polymer through a 10-20 micron filter medium, vacuum defoaming to obtain a wiredrawing spinning or precipitating polymer, and preserving at 10-50 ℃;
sp6: before spinning, the fiber is filtered by a filter element filter and then directly conveyed into a spinneret by a metering pump, and is sprayed out of the coagulating bath forming liquid to obtain nascent fibers;
sp7: the nascent fiber is formed again through a spraying area of forming liquid, and finally an aramid fiber finished product is obtained after multistage stretching, multistage washing, drying and high-temperature shaping;
the short cut of the colored 1313 meta-aramid polymer is a papermaking inter-stage benzene aramid short cut fiber which uses a fiber short cutter to cut aramid long fibers into 3mm-10mm surface-brooming. The meta-aramid chopped fiber with the brooming morphological characteristics can generate excellent cohesion force for the meta-aramid chopped fiber and the meta-aramid fibrid, and the meta-aramid chopped fiber and the meta-aramid fibrid are entangled with each other when the paper is manufactured, so that the binding point and the binding strength are improved, the purposes of high-performance paper tensile strength and tearing strength are finally realized, and the requirements of different application fields are met.
Preferably, the filter element filter adopts a filter medium of 500-1000 mesh sintered felt.
Preferably, the spinneret is a combined spinneret, the hole diameter of the spinneret is 0.05mm-0.2mm, and the hole number of the spinneret is 12000-18000.
Preferably, the coagulation bath forming liquid is an aqueous solution of calcium chloride and dimethylacetamide, the concentration of calcium chloride in the aqueous solution of calcium chloride and dimethylacetamide is set to 40 to 60wt%, the concentration of dimethylacetamide in the aqueous solution of calcium chloride and dimethylacetamide is set to 30 to 50wt%, the concentration of water in the aqueous solution of calcium chloride and dimethylacetamide is set to 5 to 10wt%, and the temperature of the coagulation bath forming liquid is set to 100 to 200 ℃. The meta-aramid polymer is conveyed into a spinneret through a metering pump and is sprayed out into a coagulating bath forming liquid to form primary fibers, and organic solvents, namely dimethylacetamide and water, which are uniformly distributed in the primary fibers are gasified to form bubbles due to the great increase of the coagulating temperature, and the bubbles are broken from the inside of the fibers to the surface of the epidermis with lower circumferential pressure, so that the fibrillated fibers are carried out at the instant of breaking.
Preferably, the spray zone forming liquid is an aqueous solution of dimethylacetamide, the concentration of the aqueous solution of dimethylacetamide is 20-60 wt%, and the temperature of the spray zone forming liquid is 0-20 ℃.
Preferably, the stretching liquid in the multistage stretching is an aqueous solution of dimethylacetamide, the concentration of the aqueous solution of dimethylacetamide is set to 20-50 wt%, and the temperature of the stretching liquid is set to 0-20 ℃.
Preferably, the drying adopts infrared heating and drying, and the temperature of the infrared heating and drying is set to be 120-130 ℃.
Preferably, the high-temperature setting adopts an infrared setting furnace, and the temperature of the infrared setting furnace is set to 320-350 ℃.
The beneficial effects of the invention are as follows:
in the invention, meta-aramid polymer is conveyed into a spinneret through a metering pump during a spinning solidification process, and is sprayed out into a primary fiber in a solidification bath forming liquid, so that organic solvent dimethylacetamide and water which are uniformly distributed in the primary fiber are gasified to form bubbles due to the great increase of solidification temperature, the bubbles are broken from the inside of the fiber to the surface of the surface with lower circumferential pressure, and the fibrillated fiber is carried out at the breaking moment. In order to obtain better performance and uniform distribution of the fibrillated fibers on the primary fibers of the body, and maintain the structural damage of the primary fibers of the body to influence the performance reduction due to the fibrillation, the forming time of the fibers in a coagulating bath is prolonged to 1-5min, so that the coagulating process is slowly and uniformly carried out, better coagulating effect is obtained, the meta-aramid fiber strength of a papermaking-grade finished product is kept to be more than 3.8cn/dtex, and meanwhile, the meta-aramid fiber strength has more excellent cohesion, is entangled with each other when paper is manufactured, the bonding point and the bonding strength are improved, the purposes of high-performance paper tensile strength and tearing strength are finally realized, and the requirements of different application fields are met.
Drawings
FIG. 1 is a flow chart of the surface fibrillation of the papermaking-grade meta-aramid fiber of the present invention;
FIG. 2 is a flow chart of the spinning of colored 1313 meta-aramid polymer of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but 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.
Examples:
as shown in fig. 1 to 2, the embodiment of the invention provides a preparation method for surface fibrillation of a paper-making-grade meta-aramid fiber, which aims to solve the problems of uneven coloring, low coloring efficiency, low color fastness of post-dyeing and limited application field of the conventional colored fiber of meta-aramid fiber before spinning.
In order to achieve the above object, the present invention provides the following technical solutions: the preparation method of the paper-making grade meta-aramid fiber surface brooming comprises the steps of synthesis, neutralization, spinning and chopping of colored 1313 meta-aramid polymer, wherein the synthesis of the colored 1313 meta-aramid polymer comprises the following steps:
sp1: m-phenylenediamine is dissolved in amide polar organic solvent DMAC;
sp2: controlling the reaction temperature to be-10 ℃ to 0 ℃, and adding the corresponding amount of 90wt% to 95wt% of isophthaloyl dichloride to carry out low-temperature polycondensation reaction;
sp3: adding a colored pigment, and adding 5-10wt% of isophthaloyl dichloride with the residual corresponding amount to continue the low-temperature polycondensation reaction;
sp4: the byproduct hydrogen chloride is subjected to a neutralization reaction by adopting alkaline earth metal oxide, hydroxide or ammonia gas, and the temperature of the neutralization reaction is controlled to be lower than 30 ℃; the concentration of the obtained meta-aramid polymer is 15-25 wt%, eta is 1.7-2.5, and the pH value is 4-7;
spinning of the colored 1313 meta-aramid polymer comprises the steps of:
sp5: filtering meta-aramid polymer through a 10-20 micron filter medium, vacuum defoaming to obtain a wiredrawing spinning or precipitating polymer, and preserving at 10-50 ℃;
sp6: before spinning, the filter element filter is made of 500-1000 mesh sintered felt. The filtered water is directly conveyed into a spinneret through a metering pump, the spinneret is set as a combined spinneret, the aperture of the spinneret is set to be 0.05mm-0.2mm, and the aperture number of the spinneret is set to be 12000-18000. Spraying the primary fiber into the coagulating bath forming liquid to obtain primary fiber; the coagulating bath forming liquid is an aqueous solution of calcium chloride and dimethylacetamide, the concentration of calcium chloride in the aqueous solution of calcium chloride and dimethylacetamide is set to 40 to 60wt%, the concentration of dimethylacetamide in the aqueous solution of calcium chloride and dimethylacetamide is set to 30 to 50wt%, the concentration of water in the aqueous solution of calcium chloride and dimethylacetamide is set to 5 to 10wt%, and the temperature of the coagulating bath forming liquid is set to 100 to 200 ℃. The meta-aramid polymer is conveyed into a spinneret through a metering pump and is sprayed out into a coagulating bath forming liquid to form primary fibers, and organic solvents, namely dimethylacetamide and water, which are uniformly distributed in the primary fibers are gasified to form bubbles due to the great increase of the coagulating temperature, and the bubbles are broken from the inside of the fibers to the surface of the epidermis with lower circumferential pressure, so that the fibrillated fibers are carried out at the instant of breaking. In order to obtain better performance and uniform distribution of the fibrillated fibers on the primary fibers of the body, and maintain the structural damage of the primary fibers of the body to influence the performance reduction due to the fibrillation, the forming time of the fibers in a coagulating bath is prolonged to 1-5min, so that the coagulating process is slowly and uniformly carried out, better coagulating effect is obtained, and the meta-aramid fiber strength of a papermaking-grade finished product is kept to be more than 3.8cn/dtex and simultaneously more excellent cohesion is provided.
Sp7: the nascent fiber is formed again through a spraying area of forming liquid, the forming liquid of the spraying area is water solution of dimethylacetamide, the concentration of the water solution of dimethylacetamide is 20-60 wt%, and the temperature of the forming liquid of the spraying area is 0-20 ℃. Through multistage stretching, the stretching liquid in the multistage stretching is set as an aqueous solution of dimethylacetamide, the concentration of the aqueous solution of dimethylacetamide is set to be 20-50 wt%, the temperature of the stretching liquid is set to be 0-20 ℃, multistage water washing and drying are carried out, infrared heating and drying are adopted for drying, and the temperature of infrared heating and drying is set to be 120-130 ℃; and (3) high-temperature setting, wherein an infrared setting furnace is adopted for the high-temperature setting, the temperature of the infrared setting furnace is set to 320-350 ℃, and finally, an aramid fiber finished product is obtained.
The short cut of the colored 1313 meta-aramid polymer is a papermaking inter-stage aramid short cut fiber with a fiber short cutter cutting the aramid long fiber into 3mm-10mm surface-fibrillated. The meta-aramid chopped fiber with the brooming morphological characteristics can generate excellent cohesion force for the meta-aramid chopped fiber and the meta-aramid fibrid, and the meta-aramid chopped fiber and the meta-aramid fibrid are entangled with each other when the paper is manufactured, so that the binding point and the binding strength are improved, the purposes of high-performance paper tensile strength and tearing strength are finally realized, and the requirements of different application fields are met.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (8)

1. The preparation method of the paper-making grade meta-aramid fiber surface brooming comprises the steps of synthesis, neutralization, spinning and chopping of colored 1313 meta-aramid polymer, wherein the synthesis of the colored 1313 meta-aramid polymer comprises the following steps:
sp1: m-phenylenediamine is dissolved in amide polar organic solvent DMAC;
sp2: controlling the reaction temperature to be-10 ℃ to 0 ℃, and adding the corresponding amount of 90wt% to 95wt% of isophthaloyl dichloride to carry out low-temperature polycondensation reaction;
sp3: adding a colored pigment, and adding 5-10wt% of isophthaloyl dichloride with the residual corresponding amount to continue the low-temperature polycondensation reaction;
sp4: the byproduct hydrogen chloride is subjected to a neutralization reaction by adopting alkaline earth metal oxide, hydroxide or ammonia gas, and the temperature of the neutralization reaction is controlled to be lower than 30 ℃;
the method is characterized in that: the spinning of the colored 1313 meta-aramid polymer comprises the following steps:
sp5: filtering meta-aramid polymer through a 10-20 micron filter medium, vacuum defoaming to obtain a wiredrawing spinning or precipitating polymer, and preserving at 10-50 ℃;
sp6: before spinning, the fiber is filtered by a filter element filter and then directly conveyed into a spinneret by a metering pump, and is sprayed out of the coagulating bath forming liquid to obtain nascent fibers;
sp7: the nascent fiber is formed again through a spraying area of forming liquid, and finally an aramid fiber finished product is obtained after multistage stretching, multistage washing, drying and high-temperature shaping;
the short cut of the colored 1313 meta-aramid polymer is a papermaking inter-stage benzene aramid short cut fiber which uses a fiber short cutter to cut aramid long fibers into 3mm-10mm surface-brooming.
2. The method for preparing the surface broom of the paper grade meta-aramid fiber, which is characterized in that: the filter medium adopted by the filter element filter is 500-1000 mesh sintered felt.
3. The method for preparing the surface broom of the paper grade meta-aramid fiber, which is characterized in that: the spinneret is a combined spinneret, the aperture of the spinneret is 0.05mm-0.2mm, and the number of holes of the spinneret is 12000-18000.
4. The method for preparing the surface broom of the paper grade meta-aramid fiber, which is characterized in that: the coagulating bath forming liquid is an aqueous solution of calcium chloride and dimethylacetamide, the concentration of the calcium chloride in the aqueous solution of the calcium chloride and dimethylacetamide is 40-60 wt%, the concentration of the dimethylacetamide in the aqueous solution of the calcium chloride and dimethylacetamide is 30-50 wt%, the concentration of the water in the aqueous solution of the calcium chloride and dimethylacetamide is 5-10 wt%, and the temperature of the coagulating bath forming liquid is 100-200 ℃.
5. The method for preparing the surface broom of the paper grade meta-aramid fiber, which is characterized in that: the forming liquid in the spraying area is an aqueous solution of dimethylacetamide, the concentration of the aqueous solution of dimethylacetamide is set to be 20-60 wt%, and the temperature of the forming liquid in the spraying area is set to be 0-20 ℃.
6. The method for preparing the surface broom of the paper grade meta-aramid fiber, which is characterized in that: the stretching liquid in the multistage stretching is an aqueous solution of dimethylacetamide, the concentration of the aqueous solution of dimethylacetamide is set to be 20-50 wt%, and the temperature of the stretching liquid is set to be 0-20 ℃.
7. The method for preparing the surface broom of the paper grade meta-aramid fiber, which is characterized in that: the drying adopts infrared heating and drying, and the temperature of the infrared heating and drying is set to be 120-130 ℃.
8. The method for preparing the surface broom of the paper grade meta-aramid fiber, which is characterized in that: the high-temperature setting adopts an infrared setting furnace, and the temperature of the infrared setting furnace is set to 320-350 ℃.
CN202311278861.1A 2023-10-06 2023-10-06 Preparation method of paper-making-grade meta-aramid fiber surface brooming Pending CN117306013A (en)

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CN202311278861.1A CN117306013A (en) 2023-10-06 2023-10-06 Preparation method of paper-making-grade meta-aramid fiber surface brooming

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Application Number Priority Date Filing Date Title
CN202311278861.1A CN117306013A (en) 2023-10-06 2023-10-06 Preparation method of paper-making-grade meta-aramid fiber surface brooming

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