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CN116516515A - Preparation method of boron nitride modified polyphenylene sulfide fiber and product thereof - Google Patents

Preparation method of boron nitride modified polyphenylene sulfide fiber and product thereof Download PDF

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Publication number
CN116516515A
CN116516515A CN202310576781.8A CN202310576781A CN116516515A CN 116516515 A CN116516515 A CN 116516515A CN 202310576781 A CN202310576781 A CN 202310576781A CN 116516515 A CN116516515 A CN 116516515A
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Prior art keywords
boron nitride
polyphenylene sulfide
fiber
modified
carrying
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CN202310576781.8A
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Chinese (zh)
Inventor
杨青山
任冰涛
高建平
李曰斌
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Shandong Minghua New Material Co ltd
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Shandong Minghua New Material Co ltd
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Priority to CN202310576781.8A priority Critical patent/CN116516515A/en
Publication of CN116516515A publication Critical patent/CN116516515A/en
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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
    • D01D5/08Melt 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
    • D01D10/00Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/02Heat treatment
    • 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
    • D01D5/08Melt spinning methods
    • D01D5/088Cooling filaments, threads or the like, leaving the spinnerettes
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • 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
    • D01F6/94Monocomponent 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 other polycondensation products
    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02GCRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G1/00Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
    • D02G1/12Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics using stuffer boxes
    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02GCRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G1/00Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
    • D02G1/20Combinations of two or more of the above-mentioned operations or devices; After-treatments for fixing crimp or curl
    • D02G1/205After-treatments for fixing crimp or curl
    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02JFINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J1/00Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
    • D02J1/22Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
    • D02J1/228Stretching in two or more steps, with or without intermediate steps
    • 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)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)

Abstract

The invention discloses a preparation method of boron nitride modified polyphenylene sulfide fibers and products thereof, belonging to the technical field of special fiber manufacturing. The preparation method comprises the steps of firstly modifying boron nitride powder by using a silane coupling agent, then mixing modified boron nitride with polyphenylene sulfide resin to obtain modified resin, then carrying out melt spinning, and obtaining formed fibers through heat setting, slow cooling area and cooling air solidification; the method comprises the steps of oiling formed fibers, winding, carrying out two-stage drafting and shaping, feeding the fibers into a crimping machine through a steam preheating box, carrying out relaxation heat shaping on the fibers, and cooling to obtain finished products. The modified polyphenylene sulfide fiber is obtained by taking the fiber-grade polyphenylene sulfide resin and boron nitride as raw materials through a melting-stretching process, and has no harsh reaction conditions. Boron nitride has excellent chemical corrosion resistance and oxidation resistance. The unique advantages of the polyphenylene sulfide fiber are utilized, and the oxidation resistance of the polyphenylene sulfide fiber is enhanced.

Description

Preparation method of boron nitride modified polyphenylene sulfide fiber and product thereof
Technical Field
The invention belongs to the technical field of special fiber manufacturing, and particularly relates to a preparation method of boron nitride modified polyphenylene sulfide fiber and a product thereof.
Background
Polyphenylene sulfide fibers (Polyphenylene Sulfide Fibre, PPS fibers) are a novel specialty plastic fiber, known by the foreign trade name, lyton (Ryton). Is prepared from polyphenylene sulfide resin (PPS) by conventional melt spinning method, and then post-stretching, crimping and cutting at high temperature. The short fiber has high strength, excellent heat stability and flame retardance, an oxygen index value of 34-35, a strength retention rate of 60% at 200 ℃, and no change in elongation at break; chemical resistance is inferior to Polytetrafluoroethylene (PTFE) fibers; has better textile processing performance. The product is mainly used for filtering high-temperature flue gas and special heat medium, drying belt in paper industry, cable wrapping adhesive layer, fireproof fabric and the like, and the woven fabric can be used for manufacturing advanced fire-fighting clothing.
However, in the using process of the PPS fiber, the temperature is higher than 180 ℃ because of the PPS macromolecular structure, the fiber can be subjected to serious oxidation phenomenon, the strength loss of the dust removal bag can reach 30% -55%, the using condition of the dust removal bag can not be met, and the effect and the service life of the dust removal bag are greatly reduced.
The boron nitride has excellent chemical corrosion resistance and oxidation resistance, and can improve the oxidation resistance of PPS fibers. Therefore, the research on the boron nitride silicon doped PPS fiber improves the oxidation resistance of the PPS fiber so as to obtain the PPS fiber with more practical performance in the aspect of dust removal bags, and has very important research value.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a preparation method of boron nitride modified polyphenylene sulfide fibers and a product thereof.
In order to achieve the above object, the present invention provides the following solutions:
the invention aims at providing a preparation method of boron nitride modified polyphenylene sulfide fibers, which comprises the following steps:
(1) Mixing boron nitride powder and a silane coupling agent in a high-speed mixer for 20-30 min at 15000-30000 r/min to obtain modified boron nitride; mixing the modified boron nitride and the polyphenylene sulfide resin in a high-speed centrifuge at 20000-30000 r/min for 20-30 min, and drying to obtain modified resin;
(2) Carrying out melt spinning on the modified resin at 300-330 ℃, then carrying out heat setting at 160-210 ℃, then passing through a slow cooling zone at 150-190 ℃, and then carrying out solidification by cooling air at 40-60 ℃ to obtain a formed fiber;
(3) And (3) oiling the formed fiber, winding, performing two-stage drafting and shaping, regulating and controlling the fiber through an amplitude modulation frame, entering a crimping machine through a steam preheating box, uniformly spreading the fiber which is discharged from the crimping machine on a link plate of a relaxation heat shaping machine under the action of a conveying yarn swinging machine, wherein the relaxation heat shaping temperature is 120-160 ℃, and cooling through forced air to obtain a finished product.
Further, the dosage of the silane coupling agent in the step (1) is 0.7-2.1% of the mass of the boron nitride powder, the boron nitride powder is a commercial product, and the mesh number is 10000-12000 mesh; the dosage of the modified boron nitride is 1-3% of the mass of the polyphenylene sulfide resin.
Further, the polyphenylene sulfide resin is a linear resin, and the melt index is 100-300 g/10min;
the silane coupling agent is a commercial product, and the molecular formula is RSiX 3 Wherein R represents amino, vinyl, epoxy, methylpropaneacyloxy, etc., and X represents a hydrolyzable group such as halogen, alkoxy, acyloxy, etc.
Further, the drying in the step (1) is vacuum drying, and the conditions of the vacuum drying are as follows: the temperature is 70-160 ℃, the vacuum degree is minus 0.06-minus 0.1MPa, and the time is 12-14 h.
Further, in the step (2), the modified resin is fed into a spinneret plate by a metering pump at a flow rate of 213.3-600 g/min, the aperture of the spinneret plate is 0.2-0.5 mm, the number of holes of the spinneret plate is 1600 holes, and the spinning speed is 600-1000 m/min.
Further, the winding speed in the step (3) is 600-1000 m/min.
Further, the two-stage drafting and sizing conditions in the step (3) are as follows: the first draft is 1.5-2, the draft speed is 150-200 m/min, the oil bath temperature is 80-120 ℃, the second draft is 1-1.5, the draft speed is 100-150 m/min, the superheated steam temperature is 120-200 ℃, and the fiber with the linear density of 2.2-2.22 dtex is obtained.
The second purpose of the invention is to provide the boron nitride modified polyphenylene sulfide fiber prepared by the preparation method.
There are no optional steps and alternative means in the above steps.
The invention has the beneficial effects that:
the modified polyphenylene sulfide fiber is obtained by taking the fiber-grade polyphenylene sulfide resin and boron nitride as raw materials through a melting-stretching process, and has no harsh reaction conditions. Boron nitride has excellent chemical corrosion resistance and oxidation resistance. The unique advantages of the polyphenylene sulfide fiber are utilized, and the oxidation resistance of the polyphenylene sulfide fiber is enhanced.
Detailed Description
The present invention will be described in further detail with reference to examples for better understanding of the technical scheme of the present invention to those skilled in the art.
Example 1
(1) Mixing boron nitride powder with a silane coupling agent at 15000r/min for 20min to obtain modified boron nitride; mixing the modified boron nitride with polyphenylene sulfide resin for 20min at 20000r/min, and vacuum drying to obtain modified resin, wherein the vacuum drying conditions are as follows: the temperature is 70 ℃, the vacuum degree is-0.06 MPa, and the time is 12 hours;
the dosage of the silane coupling agent is 0.7% of the mass of the boron nitride powder, and the mesh number of the boron nitride powder is 10000 mesh; the dosage of the modified boron nitride is 1% of the mass of the polyphenylene sulfide resin, the polyphenylene sulfide resin is linear resin, and the melt index is 100g/10min;
(2) Feeding the modified resin into a spinneret plate by a metering pump at a flow rate of 213.3g/min, wherein the melting temperature is 300 ℃, the aperture of the spinneret plate is 0.2mm, the number of the spinneret plate holes is 1600 holes, the spinning speed is 600m/min, carrying out melt spinning, then carrying out heat setting at 160 ℃, then passing through a slow cooling zone at 150 ℃, and then carrying out curing at 40 ℃ by cooling air to obtain a molded fiber;
(3) Oiling the formed fiber, winding at the speed of 750m/min, and performing two-stage drafting and shaping: the primary draft multiple is 1.5, the draft speed is 150m/min, the oil bath temperature is 80 ℃, the secondary draft multiple is 1, the draft speed is 100m/min, the superheated steam temperature is 120 ℃, and the fiber with the linear density of 2.22dtex is obtained.
And then the fibers are regulated and controlled by an amplitude modulation frame and enter a crimping machine through a steam preheating box, the crimping temperature is 120 ℃, the fibers which are discharged from the crimping machine are evenly paved on a link plate of a relaxation heat setting machine under the action of a conveying yarn swinging machine, the relaxation heat setting temperature is 120 ℃, and the finished product is obtained after forced air cooling.
After passing through a wire guide frame and a traction tension machine, the product is fed into a cutter from the tangential direction of a horizontally placed cutter head under uniform tension, the cutting length is 51mm, the product is distributed into a packer, and the product is compressed into bags, wherein the weight of each bag is 250kg.
And (3) product inspection: the boron nitride modified polyphenylene sulfide fiber was sent to a third party detection agency (Shandong Ming's new materials Co., ltd.) for comparative detection of the antioxidant capacity of the product fiber, and the results are shown in Table 1.
TABLE 1
Example 2
(1) Mixing boron nitride powder with a silane coupling agent at 20000r/min for 25min to obtain modified boron nitride; mixing the modified boron nitride with polyphenylene sulfide resin at 25000r/min for 25min, and vacuum drying to obtain modified resin, wherein the vacuum drying conditions are as follows: the temperature is 115 ℃, the vacuum degree is-0.08 MPa, and the time is 13h;
the dosage of the silane coupling agent is 1% of the mass of the boron nitride powder, and the mesh number of the boron nitride powder is 15000 mesh; the dosage of the modified boron nitride is 1.5% of the mass of the polyphenylene sulfide resin, the polyphenylene sulfide resin is linear resin, and the melt index is 200g/10min;
(2) Feeding the modified resin into a spinneret plate by a metering pump at a flow rate of 550g/min, wherein the melting temperature is 320 ℃, the aperture of the spinneret plate is 0.4mm, the number of the spinneret plate holes is 1600 holes, carrying out melt spinning under the condition that the spinning speed is 800m/min, carrying out heat setting at 180 ℃, then passing through a slow cooling zone at 170 ℃, and then carrying out curing at 50 ℃ by cooling air to obtain a molded fiber;
(3) Oiling the formed fiber, winding at 825m/min, and performing two-stage drafting and shaping: the primary draft multiple is 1.75, the draft speed is 175m/min, the oil bath temperature is 100 ℃, the secondary draft multiple is 1.25, the draft speed is 125m/min, the superheated steam temperature is 150 ℃, and the fiber with the linear density of 2.2dtex is obtained.
And then the fibers are regulated and controlled by an amplitude modulation frame and enter a crimping machine through a steam preheating box, the crimping temperature is 200 ℃, the fibers which are discharged from the crimping machine are evenly paved on a link plate of a relaxation heat setting machine under the action of a conveying yarn swinging machine, the relaxation heat setting temperature is 140 ℃, and the finished product is obtained after forced air cooling.
After passing through a wire guide frame and a traction tension machine, the product is fed into a cutter from the tangential direction of a horizontally placed cutter head under uniform tension, the cutting length is 51mm, the product is distributed into a packer, and the product is compressed into bags, wherein the weight of each bag is 250kg.
And (3) product inspection: the boron nitride modified polyphenylene sulfide fiber was sent to a third party detection agency (Shandong Ming's New Material Co., ltd.) for comparative detection of the antioxidant capacity of the product fiber, and the results are shown in Table 2.
TABLE 2
Example 3
(1) Mixing boron nitride powder with a silane coupling agent for 30min at 30000r/min to obtain modified boron nitride; mixing the modified boron nitride with polyphenylene sulfide resin for 30min at 30000r/min, and vacuum drying to obtain modified resin, wherein the vacuum drying conditions are as follows: the temperature is 160 ℃, the vacuum degree is-0.1 MPa, and the time is 14 hours;
the dosage of the silane coupling agent is 2.1 percent of the mass of the boron nitride powder, and the mesh number of the boron nitride powder is 12000 meshes; the dosage of the modified boron nitride is 3% of the mass of the polyphenylene sulfide resin, the polyphenylene sulfide resin is linear resin, and the melt index is 300g/10min;
(2) Feeding the modified resin into a spinneret plate by a metering pump at a flow rate of 600g/min, wherein the melting temperature is 330 ℃, the aperture of the spinneret plate is 0.5mm, the number of the spinneret plate holes is 1600 holes, carrying out melt spinning under the condition that the spinning speed is 1000m/min, then carrying out heat setting at 210 ℃, then passing through a slow cooling zone at 190 ℃, and then carrying out curing at 60 ℃ by cooling air to obtain a molded fiber;
(3) Oiling the formed fiber, winding at the winding speed of 900m/min, and performing two-stage drafting and shaping: the primary draft multiple is 2, the draft speed is 200m/min, the oil bath temperature is 120 ℃, the secondary draft multiple is 1.5, the draft speed is 150m/min, the superheated steam temperature is 200 ℃, and the fiber with the linear density of 2.2dtex is obtained.
And then the fibers are regulated and controlled by an amplitude modulation frame and enter a crimping machine through a steam preheating box, the crimping temperature is 240 ℃, the fibers which are discharged from the crimping machine are evenly paved on a link plate of a relaxation heat setting machine under the action of a conveying yarn swinging machine, the relaxation heat setting temperature is 160 ℃, and the finished product is obtained after forced air cooling.
After passing through a wire guide frame and a traction tension machine, the product is fed into a cutter from the tangential direction of a horizontally placed cutter head under uniform tension, the cutting length is 51mm, the product is distributed into a packer, and the product is compressed into bags, wherein the weight of each bag is 250kg.
And (3) product inspection: the boron nitride modified polyphenylene sulfide fiber was sent to a third party detection agency (Shandong Ming's New Material Co., ltd.) for comparative detection of the antioxidant capacity of the product fiber, and the results are shown in Table 3.
TABLE 3 Table 3
As can be seen from tables 1 to 3, the modified polyphenylene sulfide fiber is obtained by using the fiber-grade polyphenylene sulfide resin and boron nitride as raw materials through a melting-stretching process, and under the action of different oxidants, the retention rate of the modified polyphenylene sulfide fiber is obviously improved compared with that of the unmodified polyphenylene sulfide fiber, so that the oxidation resistance of the polyphenylene sulfide fiber can be enhanced by the modification method.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.

Claims (7)

1. The preparation method of the boron nitride modified polyphenylene sulfide fiber is characterized by comprising the following steps of:
(1) Mixing boron nitride powder with a silane coupling agent for 20-30 min at 15000-30000 r/min to obtain modified boron nitride; mixing the modified boron nitride with polyphenylene sulfide resin for 20-30 min at 20000-30000 r/min, and drying to obtain modified resin;
(2) Carrying out melt spinning on the modified resin at 300-330 ℃, then carrying out heat setting at 160-210 ℃, then passing through a slow cooling zone at 150-190 ℃, and then carrying out solidification by cooling air at 40-60 ℃ to obtain a formed fiber;
(3) And (3) oiling the formed fiber, winding, carrying out two-stage drafting and shaping, then feeding the fiber into a crimping machine through a steam preheating box, carrying out relaxation heat shaping on the fiber at 120-240 ℃, and cooling to obtain a finished product.
2. The preparation method according to claim 1, wherein the silane coupling agent in the step (1) is used in an amount of 0.7-2.1% by mass of boron nitride powder, and the mesh number of the boron nitride powder is 10000-12000 mesh; the dosage of the modified boron nitride is 1-3% of the mass of the polyphenylene sulfide resin.
3. The method of claim 1, wherein the drying in step (1) is vacuum drying under the following conditions: the temperature is 70-160 ℃, the vacuum degree is minus 0.06-minus 0.1MPa, and the time is 12-14 h.
4. The method according to claim 1, wherein the melt spinning in the step (2) is carried out by feeding the modified resin into a spinneret plate at a flow rate of 213.3-600 g/min by a metering pump, wherein the diameter of the spinneret plate is 0.2-0.5 mm, the number of the spinneret plate holes is 1600 holes, and the spinning speed is 600-1000 m/min.
5. The method according to claim 1, wherein the winding speed in the step (3) is 600 to 1000m/min.
6. The method of claim 1, wherein the two-stage drawing and sizing conditions of step (3) are: the first draft is 1.5-2, the draft speed is 150-200 m/min, the oil bath temperature is 80-120 ℃, the second draft is 1-1.5, the draft speed is 100-150 m/min, the superheated steam temperature is 120-200 ℃, and the fiber with the linear density of 2.2-2.22 dtex is obtained.
7. A boron nitride modified polyphenylene sulfide fiber produced by the production process according to any one of claims 1 to 6.
CN202310576781.8A 2023-05-22 2023-05-22 Preparation method of boron nitride modified polyphenylene sulfide fiber and product thereof Pending CN116516515A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118308803A (en) * 2024-06-05 2024-07-09 天津市凯瑞新材料科技有限公司 Preparation method of modified polyphenylene sulfide fiber

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118308803A (en) * 2024-06-05 2024-07-09 天津市凯瑞新材料科技有限公司 Preparation method of modified polyphenylene sulfide fiber

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