CN111235668A - Method for preparing ultra-high molecular weight polyethylene fiber and fiber - Google Patents
Method for preparing ultra-high molecular weight polyethylene fiber and fiber Download PDFInfo
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- CN111235668A CN111235668A CN202010264680.3A CN202010264680A CN111235668A CN 111235668 A CN111235668 A CN 111235668A CN 202010264680 A CN202010264680 A CN 202010264680A CN 111235668 A CN111235668 A CN 111235668A
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- 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
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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- 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
- D01D10/02—Heat treatment
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- 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
- D01D5/08—Melt spinning methods
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- 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
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
-
- 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
- D01D5/12—Stretch-spinning methods
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- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- Chemical Kinetics & Catalysis (AREA)
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- Artificial Filaments (AREA)
Abstract
The invention discloses a method for manufacturing ultra-high molecular weight polyethylene fibers and the fibers, and relates to the technical field of high-strength fiber materials. A method for making ultra-high molecular weight polyethylene fibers, the method comprising the steps of: uniformly mixing the ultrahigh molecular weight polyethylene powder with white oil and a nanoscale nucleating agent, and heating and pre-swelling in a reaction kettle to obtain a mixed system; feeding the mixed system into a co-rotating double-screw extruder for melt spinning, carrying out spinneret plate and traction, and carrying out chilled water cooling cutting to obtain gel fibers; pre-drafting, extracting and drying the gel fiber, and then carrying out three-stage hot drafting to obtain a strong ultrahigh molecular weight polyethylene fiber; wherein the ultra-high molecular weight polyethylene powder is an ultra-high molecular weight polyethylene resin having a molecular weight of 800 to 1200 ten thousand. The prepared ultra-high molecular weight polyethylene fiber has high strength.
Description
Technical Field
The invention relates to the technical field of high-strength fiber materials, in particular to a method for manufacturing ultra-high molecular weight polyethylene fibers and the fibers.
Background
The ultra-high molecular weight polyethylene fiber is also called high-strength high-modulus polyethylene fiber, is the fiber with the highest specific strength and specific modulus in the world at present, and is the fiber spun by polyethylene with the molecular weight of 100-500 ten thousand. Since the key production technology of the ultra-high molecular weight polyethylene fiber is broken in the same year and in the same year of 1994, a plurality of industrial production bases for the ultra-high molecular weight polyethylene fiber are formed in China. It is reported that 70% of the U.S. ultrahigh molecular weight polyethylene fiber is used in the military fields of body armor, bulletproof helmet, bulletproof armor of military facilities and equipment, aerospace and the like, and the development of high performance fiber is an embodiment of the comprehensive strength of the country and is an important material foundation for building modernized strong countries.
With the wider application of high-strength polyethylene, especially the application in the aspect of light-weight bulletproof materials, the requirement on the strong temperature of the fiber is higher and higher.
Disclosure of Invention
The present invention aims to provide a method for producing an ultra-high molecular weight polyethylene fiber and a fiber, so as to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme:
in one aspect, a method for making ultra-high molecular weight polyethylene fibers, the method comprising the steps of:
uniformly mixing the ultrahigh molecular weight polyethylene powder with white oil and a nanoscale nucleating agent, and heating and pre-swelling in a reaction kettle to obtain a mixed system;
feeding the mixed system into a co-rotating double-screw extruder for melt spinning, carrying out spinneret plate and traction, and carrying out chilled water cooling cutting to obtain gel fibers;
pre-drafting, extracting and drying the gel fiber, and then carrying out three-stage hot drafting to obtain a strong ultrahigh molecular weight polyethylene fiber;
wherein the ultra-high molecular weight polyethylene powder is an ultra-high molecular weight polyethylene resin having a molecular weight of 800 to 1200 ten thousand.
Preferably, the weight ratio of the ultra-high molecular weight polyethylene powder is 6-12%, the weight ratio of the nano nucleating agent is 0.1-0.5%, and the balance is white oil.
Preferably, the nano nucleating agent is dbs, aryl phosphate ester salt or nano titanium dioxide.
Preferably, the temperature of the co-rotating twin screw is 100-250 ℃.
Preferably, the temperature of the screw feeding section of the co-rotating twin screw is 120-180 ℃, the temperature of the compression shearing section is 190-250 ℃, and the temperature of the homogenization output section is 240-250 ℃.
Preferably, the temperature of the frozen water-cooled cutting is 5-12 ℃.
Preferably, the three-stage hot drawing temperature is 140-155 ℃, and the total drawing multiple is 60-80 times.
Preferably, the temperature of the three-stage hot drawing is 145-148 ℃, 152-154 ℃ and 150-155 ℃;
preferably, the reaction kettle is heated and pre-swelled to 115-118 ℃ to obtain a mixed system.
On the other hand, the invention also provides the ultra-high molecular weight polyethylene fiber which is prepared by adopting any one of the preparation methods.
Compared with the prior art, the invention has the beneficial effects that:
the invention adds the nanometer nucleating agent into the system of the ultra-high molecular weight polyethylene and the white oil, the nucleating agent adopts nanometer materials and is evenly distributed in the system, in the hot drawing of the ultra-high molecular weight polyethylene fiber, the crystal nucleus can promote the crystallization degree of the ultra-high molecular weight polyethylene fiber to be higher and the crystallization to be more compact through induced crystallization, simultaneously improves the orientation degree of the distribution of the chain segment of the ultra-high molecular weight polyethylene fiber, and can obviously increase the strength, the modulus, the melting point and the like of the ultra-high molecular weight polyethylene fiber. The prepared ultra-high molecular weight polyethylene fiber has high strength.
Detailed Description
In order to enhance the understanding of the present invention, the present invention will be further described with reference to the following examples, which are only for the purpose of illustrating the present invention and are not to be construed as limiting the scope of the present invention.
The embodiment of the invention provides, on the one hand, a manufacturing method of an ultrahigh molecular weight polyethylene fiber, which comprises the following steps:
uniformly mixing the ultrahigh molecular weight polyethylene powder with white oil and a nanoscale nucleating agent, and heating and pre-swelling in a reaction kettle to obtain a mixed system;
feeding the mixed system into a co-rotating double-screw extruder for melt spinning, carrying out spinneret plate and traction, and carrying out chilled water cooling cutting to obtain gel fibers;
pre-drafting, extracting and drying the gel fiber, and then carrying out three-stage hot drafting to obtain a strong ultrahigh molecular weight polyethylene fiber;
wherein the ultra-high molecular weight polyethylene powder is an ultra-high molecular weight polyethylene resin having a molecular weight of 800 to 1200 ten thousand.
In the above embodiment, a trace amount of nucleating agent is added into the system of ultra-high molecular weight polyethylene and mineral white oil, the nucleating agent is a nano-scale material and is uniformly distributed in the system, and in the hot drawing of the ultra-high strength and ultra-high molecular weight polyethylene fiber, the crystallization nuclei can promote the high crystallinity and the denser crystallization of the ultra-high molecular weight polyethylene fiber through induced crystallization, and simultaneously, the orientation degree of the distribution of the chain segments of the ultra-high molecular weight polyethylene fiber is improved, so that the strength, modulus, melting point and the like of the ultra-high molecular weight polyethylene fiber can be remarkably increased.
In one embodiment, the weight ratio of the ultra-high molecular weight polyethylene powder is 6-12%, the weight ratio of the nano-scale nucleating agent is 0.1-0.5%, and the balance is white oil. The ultra-high molecular weight polyethylene resin and the mineral white oil are blended and extruded, the white oil is one or a mixture of 50# and 70# and the concentration of the ultra-high molecular weight polyethylene is controlled to be 6-12%, so that the melt fluidity can be well ensured, and the production stability and uniformity are ensured.
In one embodiment, the nano nucleating agent is dbs, aryl phosphate or nano titanium dioxide, wherein dbs is a sorbitol nucleating agent.
In one embodiment, the temperature of the co-rotating twin screws is 100-250 ℃.
In one embodiment, the temperature of the screw feeding section of the co-rotating twin screw is 120-.
In one embodiment, the chilled water cutting temperature is 5-12 ℃.
In one embodiment, the three-stage thermal stretching temperature is 140-.
In one embodiment, the temperature of the three-stage hot drawing is 145-148 ℃, 152-154 ℃, and 150-155 ℃;
in one embodiment, the reaction kettle is heated to pre-swell to 115-118 ℃ to obtain a mixed system.
On the other hand, the invention also provides the ultra-high molecular weight polyethylene fiber which is prepared by adopting any one of the preparation methods.
The following is a detailed description of the specific examples:
example 1
800 ten thousand of ultrahigh molecular weight polyethylene powder with the mass ratio of 8 percent, 91.9 percent of white oil and 0.1 percent of nano nucleating agent are uniformly mixed, and the mixture is heated and pre-swelled to 115 ℃ in a reaction kettle to obtain a mixed system. And feeding the mixed system into a co-rotating double-screw extruder for melt spinning, wherein the temperature of a screw feeding section is 180 ℃ in addition, the temperature of a compression shearing section is 190 ℃ in addition, the temperature of a homogenization output section is 240 ℃, metering is carried out by a metering pump, a spinneret plate is used for traction, and 6 ℃ chilled water is used for cold cutting to obtain the gel fiber.
Pre-drafting, extracting and drying the gel fiber, performing 3 times of hot drafting at 145 ℃, 152 ℃ and 150 ℃ respectively, wherein the total stretching multiple is 65 times, and winding to obtain the ultrahigh-strength and ultrahigh-molecular-weight polyethylene fiber with the tensile strength of 38.5cn/dtex, the tensile modulus of 1780cn/dtex and the elongation at break of 2.5%.
Example 2
Mixing 1000 ten thousand of molecular weight ultrahigh molecular weight polyethylene powder with the mass ratio of 7.5 percent, 92.3 percent of white oil and 0.2 percent of nano nucleating agent uniformly, heating and pre-swelling the mixture in a reaction kettle to 118 ℃ to obtain a mixed system. And feeding the mixed system into a co-rotating double-screw extruder for melt spinning, wherein the temperature of a screw feeding section is 180 ℃ and the temperature of a compression shearing section is 190 ℃ and 250 ℃ and the temperature of a homogenization output section is 245 ℃, metering by a metering pump, spinning a spinneret plate, drawing and cold cutting by 5 ℃ chilled water to obtain the gel fiber.
Pre-drafting, extracting and drying the gel fiber, performing 3 times of hot drafting at 145 ℃, 152 ℃ and 150 ℃ respectively, wherein the total stretching multiple is 75 times, and winding to obtain the ultrahigh-strength and ultrahigh-molecular-weight polyethylene fiber with the tensile strength of 40.5cn/dtex, the tensile modulus of 1850cn/dtex and the elongation at break of 2.4%.
Example 3
1200 million of molecular weight ultra-high molecular weight polyethylene powder with the mass ratio of 7 percent, 92.7 percent of white oil and 0.3 percent of nano nucleating agent are uniformly mixed, and the mixture is heated and pre-swelled to 115 ℃ in a reaction kettle to obtain a mixed system. And feeding the mixed system into a co-rotating double-screw extruder for melt spinning, wherein the temperature of a screw feeding section is 180 ℃ in addition, the temperature of a compression shearing section is 190 ℃ in addition, the temperature of a homogenization output section is 250 ℃, metering by a metering pump, a spinneret plate, traction and cold cutting by 7 ℃ chilled water are carried out, and the gel fiber is obtained.
Pre-drafting, extracting and drying the gel fiber, performing 3 times of hot drafting at 148 ℃, 154 ℃ and 153 ℃ respectively, wherein the total stretching multiple is 82 times, and winding to obtain the ultrahigh-strength and ultrahigh-molecular-weight polyethylene fiber with the tensile strength of 42.5cn/dtex, the tensile modulus of 1910cn/dtex and the elongation at break of 2.2%.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A manufacturing method of ultra-high molecular weight polyethylene fibers is characterized by comprising the following steps:
uniformly mixing the ultrahigh molecular weight polyethylene powder with white oil and a nanoscale nucleating agent, and heating and pre-swelling in a reaction kettle to obtain a mixed system;
feeding the mixed system into a co-rotating double-screw extruder for melt spinning, carrying out spinneret plate and traction, and carrying out chilled water cooling cutting to obtain gel fibers;
pre-drafting, extracting and drying the gel fiber, and then carrying out three-stage hot drafting to obtain a strong ultrahigh molecular weight polyethylene fiber;
wherein the ultra-high molecular weight polyethylene powder is an ultra-high molecular weight polyethylene resin having a molecular weight of 800 to 1200 ten thousand.
2. The method of claim 1, wherein the ultra-high molecular weight polyethylene powder is added in an amount of 6 to 12% by mass, the nano-sized nucleating agent is added in an amount of 0.1 to 0.5% by mass, and the balance is white oil.
3. The method of claim 1, wherein the nano-sized nucleating agent is dbs, aryl phosphate or nano-sized titanium dioxide.
4. The method for preparing ultra-high molecular weight polyethylene fiber according to claim 1, wherein the temperature of the co-rotating twin screws is 100-250 ℃.
5. The method for preparing the ultra-high molecular weight polyethylene fiber as claimed in claim 1, wherein the temperature of the screw feeding section of the co-rotating twin-screw is 120-180 ℃, the temperature of the compression shearing section is 190-250 ℃, and the temperature of the homogenization output section is 240-250 ℃.
6. The method of claim 1, wherein the temperature of the chilled water cutting is 5-12 ℃.
7. The method as claimed in claim 1, wherein the three-stage hot-drawing temperature is 140-155 ℃ and the total draw ratio is 60-80.
8. The method of claim 1, wherein the temperatures of the three-stage hot drawing are 145 to 148 ℃, 152 to 154 ℃, and 150 to 155 ℃.
9. The method for preparing the ultra-high molecular weight polyethylene fiber according to claim 1, wherein the mixed system is obtained by heating and pre-swelling in a reaction kettle to 115-118 ℃.
10. An ultra-high molecular weight polyethylene fiber produced by the production method according to any one of claims 1 to 9.
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| CN202010264680.3A CN111235668A (en) | 2020-04-07 | 2020-04-07 | Method for preparing ultra-high molecular weight polyethylene fiber and fiber |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111676570A (en) * | 2020-07-23 | 2020-09-18 | 浙江乐森科技有限公司 | Antibacterial anti-seepage fabric |
| CN113122949A (en) * | 2021-05-21 | 2021-07-16 | 浙江千禧龙纤特种纤维股份有限公司 | Ultrahigh molecular weight polyethylene fiber for manufacturing reservoir seepage-proofing paving cloth and preparation method thereof |
| CN113151912A (en) * | 2021-05-10 | 2021-07-23 | 浙江理工大学上虞工业技术研究院有限公司 | Ultra-high molecular weight polyethylene fiber and preparation method and application thereof |
| CN113293452A (en) * | 2021-03-15 | 2021-08-24 | 浙江千禧龙纤特种纤维股份有限公司 | Ultra-high molecular weight polyethylene fiber cable, cable material and preparation method thereof |
| CN113502555A (en) * | 2021-04-13 | 2021-10-15 | 山东莱威新材料有限公司 | Preparation method of ultrahigh molecular weight polyethylene fiber with strength greater than 39cN/dtex |
| CN114990915A (en) * | 2022-07-01 | 2022-09-02 | 山东莱威新材料有限公司 | Preparation method of ultrahigh molecular weight polyethylene fiber rope with strength greater than 39cN/dtex |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111676570A (en) * | 2020-07-23 | 2020-09-18 | 浙江乐森科技有限公司 | Antibacterial anti-seepage fabric |
| CN113293452A (en) * | 2021-03-15 | 2021-08-24 | 浙江千禧龙纤特种纤维股份有限公司 | Ultra-high molecular weight polyethylene fiber cable, cable material and preparation method thereof |
| CN113293452B (en) * | 2021-03-15 | 2022-06-03 | 浙江千禧龙纤特种纤维股份有限公司 | Ultra-high molecular weight polyethylene fiber cable, cable material and preparation method thereof |
| CN113502555A (en) * | 2021-04-13 | 2021-10-15 | 山东莱威新材料有限公司 | Preparation method of ultrahigh molecular weight polyethylene fiber with strength greater than 39cN/dtex |
| CN113151912A (en) * | 2021-05-10 | 2021-07-23 | 浙江理工大学上虞工业技术研究院有限公司 | Ultra-high molecular weight polyethylene fiber and preparation method and application thereof |
| CN113122949A (en) * | 2021-05-21 | 2021-07-16 | 浙江千禧龙纤特种纤维股份有限公司 | Ultrahigh molecular weight polyethylene fiber for manufacturing reservoir seepage-proofing paving cloth and preparation method thereof |
| CN114990915A (en) * | 2022-07-01 | 2022-09-02 | 山东莱威新材料有限公司 | Preparation method of ultrahigh molecular weight polyethylene fiber rope with strength greater than 39cN/dtex |
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Application publication date: 20200605 |