CN109680351A - Ultra-high molecular weight polyethylene colored fibers and preparation method thereof - Google Patents
Ultra-high molecular weight polyethylene colored fibers and preparation method thereof Download PDFInfo
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- CN109680351A CN109680351A CN201710974022.1A CN201710974022A CN109680351A CN 109680351 A CN109680351 A CN 109680351A CN 201710974022 A CN201710974022 A CN 201710974022A CN 109680351 A CN109680351 A CN 109680351A
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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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- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
Ultra-high molecular weight polyethylene colored fibers and preparation method, by polyvinyl resin with super-high molecular weight and spinning good solvent, auxiliary agent, especially specific complex antioxidant and special inorganic pigment or the mixed solution for having particular fluid rheological property of organic pigment formation, expand the ultra-high molecular weight polyethylene colored fibers that preparation excellent quality is set in trial assembly by our hospital's dry spinning, the nascent colored fibre prepared using ultra-high molecular weight polyethylene mixed solution dry spinning prepared by antioxidant, finished fiber through high power first break draft, its intensity is 10 ~ 42g/d, modulus is 300 ~ 1700g/d.
Description
Technical field
The invention belongs to chemical fiber fields, are related to a kind of raising ultra-high molecular weight polyethylene mixed solution dry spinning
The method for preparing colored fibre performance, and to ultra-high molecular weight polyethylene mixed solution compound antioxidant it is obtained have it is excellent
The ultra-high molecular weight polyethylene colored fibers of anisotropic energy.
Background technique
Ultra-high molecular weight polyethylene (UHMWPE) fiber, also known as high-strength high-modulus polyethylene fiber, it is to go out the beginning of the nineties
Existing high-tech, high-performance fiber, are three big tec fiber (carbon fiber, aramid fiber, high-strength and high-modulus polyethylene fiber of the world today
Dimension) one of, due to the dilute fiber of superhigh molecular weight polyethylene have high-crystallinity and height-oriented extended-chain configuration, with carbon fiber,
Aramid fiber compares, and the intensity of the dilute fiber of superhigh molecular weight polyethylene is higher；Quality is lighter, and chemical stability is more preferable；With very
Strong chemical inertness, resistance to strong acid, strong base solution and organic solvent；With good weatherability, after 1500h solarization, fiber is strong
Degree conservation rate is still up to 80%, and UV resistance is very superior；Lower temperature resistance is good, can be down to -150 DEG C using temperature；It
Outside, the wear-resisting resistance to bend(ing) energy of the dilute fiber of superhigh molecular weight polyethylene, fatigue tension performance, anti-cut performance are also existing high-performance
It is strongest in fiber.Act foot is played in safety, protection, Aeronautics and Astronautics, defence equipment, vehicle manufacture, shipbuilding industry, sporting world
The effect of weight.It is widely used in the fields such as rope, fishing net, setline, composite material.In addition to this, superhigh molecular weight polyethylene is dilute
Before fiber also has wide application as shock resistance, vibration-absorptive material and high performance light composite material in civilian industry field
Scape.
Since molecular weight is high, main chain is combined high-strength high-modulus polyethylene fiber, and the degree of orientation, crystallinity are high, therefore it
Specific strength is that the most polyethylene of current all fibres has methylene (- 2,6 di-tert-butyl p-cresol H2-2,6 di-t-butyls
Paracresol H2-) connected macromolecular chain chemical structure, superhigh molecular weight polyethylene is dilute, and there are the amorphous areas of a large amount of random coils
With the crystal structure of folded chain.In super times of drawing-off, macromolecular chain it is height-oriented, fill the macromolecular of crystalline region and amorphous area
Divide stretching, extension, forms the extended chain supramolecular structure of highly crystalline.Such supramolecular structure determines high-tenacity polyethylene fibre
Superior function.Its molecule is nonpolarity simultaneously and crystallization regularity is difficult to dye molecule cut wherein, and stock-dye is difficult,
Produce at present it is mostly be brown stock.If being directly mixed in inorganic pigment additive, pigment in ultra-high molecular weight polyethylene powder
Bad dispersibility easy to reunite easily causes uneven dyeing, is made into and is dyed again after product since the chemical inertness light fastness of polyethylene is not high.
Summary of the invention
Method of the invention is: provide it is a kind of produce ultra-high molecular weight polyethylene mixed solution dry spinning preparation it is coloured
Fiber and its method.
Scheme of the invention are as follows: ultra-high molecular weight polyethylene colored fibers, it is characterised in that the colored fibre is by superelevation point
What sub- weight ethylene resin and spinning good solvent, auxiliary agent and inorganic pigment or organic pigment were formed has particular fluid rheology
The mixed solution of performance, the ultra-high molecular weight polyethylene colored fibers prepared by dry spinning processes；The auxiliary agent includes anti-
Oxygen agent.
The antioxidant: four (β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol esters are (below with letter
Four (Β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol esters refer to)；(the 2,4- di-tert-butyl of phosphorous acid three
Base) ester；One of 2,6 di-tert-butyl p-cresol.
(Β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester of antioxidant four or phosphorous acid three
The additive amount of (2,4- di-tert-butyl-phenyl) ester is 0.1 ~ 2.0%wt.
(Β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester of antioxidant four or phosphorous acid three
The additive amount of (2,4- di-tert-butyl-phenyl) ester is 0.5 ~ 1.2%wt.
The antioxidant is 2,6 di-tert-butyl p-cresol.
The 2,6 di-tert-butyl p-cresol additive amount of antioxidant is 0.2 ~ 1.5%wt.
The 2,6 di-tert-butyl p-cresol additive amount of antioxidant is 0.7 ~ 1.0%wt.
Four (Β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester of antioxidant and phosphorous acid three (2,
4- di-tert-butyl-phenyl) ester compound addition range be 0.3 ~ 1.2%wt；Four (Β-(3,5- di-tert-butyl-hydroxy phenyl) third
Acid) pentaerythritol ester and phosphorous acid three (2,4- di-tert-butyl-phenyl) ester ratio range 5:1 ~ 1:5.
Four (Β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester of antioxidant and phosphorous acid three (2,
4- di-tert-butyl-phenyl) ester compound addition range be 0.5 ~ 0.9%wt, four (Β-(3,5- di-tert-butyl-hydroxy phenyl) third
Acid) pentaerythritol ester and phosphorous acid three (2,4- di-tert-butyl-phenyl) ester ratio range 3:1 ~ 1:3.
The nascent colored fibre prepared using ultra-high molecular weight polyethylene mixed solution dry spinning prepared by the present invention,
Finished fiber after high drafting, intensity are 10 ~ 42g/d, and modulus is 300 ~ 1700g/d.
The present invention targetedly instructs to spin on the basis of optimizing original spinning technique by the characterization to spinning material liquid
The preparation test of the setting and adjusting of silk process device and technological parameter, especially raising characteristic series fiber performance, i.e., it is laborsaving
Reduce unnecessary material waste, hence it is evident that reduce and expand the test production cost that trial assembly is set, and improve fiber quality.
Specific embodiment
Below by way of specific example, the present invention is further explained.It should be understood that cited example is only used for the narration present invention
Rather than it limits the scope of the invention, and not to general spinning equipment such as double screw extruder, metering in illustrated example
Pump, spinneret etc. are defined, but do not influence the preparation of the present invention excellent colored fibre obtained.In addition, it should also be understood that, readding
After the content that reader invention is lectured, those skilled in the art can make various changes or modification to the present invention, these shapes of equal value
Formula also falls within the range of the application the attached claims restriction.
Example 1
By UHMWPE resin (Relative average molecular weight is 4,500,000), 210 liters of good solvents (preferably decahydronaphthalenes), the antioxygens of 16KG
The additive amount of agent four (Β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester respectively is UHMWPE resin
0.5%, 0.7%, the 0.9% of weight is uniformly mixed by coppers, the solution in injection special raw material configuration system is twined in kettle and is swollen
It 3.5 hours, is injected in homogeneous kettle by reflux delivery pump and is further sheared, sampling carries out the fluid rheology of the mixed solution at this time
Property test, data result is shown in Table 1, and the storage tank that mixed solution passes through that band stirs later quantitatively enters double screw extruder and (cuts
For cutting speed rate for spinning equipments extruding spinnings such as 80rpm), static mixer, spinnerets, obtained frozen glue precursor passes through circular blow equipment
After the most of good solvent for including in it recycling, then optimized improved upper cluster tool and company positioned at path entrance
The winding apparatus of path outlet is connect, precursor obtains high power jet stretch, obtains the preparation of UHMWPE mixed resin solution dry spinning
Nascent colored fibre, through high power multistage first break draft obtain finished product ultra-high molecular weight polyethylene colored fibers, finished fiber is taken
Sample carries out characteristic test, and the characteristic index part such as intensity, modulus, fiber number, color fastness is shown in Table 2.
Example 2
By UHMWPE resin (Relative average molecular weight is 4,500,000), 210 liters of good solvents (preferably decahydronaphthalenes), the antioxygens of 16KG
The additive amount of agent phosphorous acid three (2,4- di-tert-butyl-phenyl) ester with this be respectively UHMWPE weight resin 0.5%, 0.7%,
0.9%, solution uniformly mixed by coppers, in injection special raw material configuration system, which twines in kettle, to be swollen 3.5 hours, passes through reflux
It is further sheared in delivery pump injection homogeneous kettle, sampling at this time carries out the fluid rheology test of the mixed solution, data knot
Fruit is shown in Table 1, and the storage tank that mixed solution passes through that band stirs later quantitatively enters double screw extruder, and (shear rate is
80rpm), the spinning equipments extruding spinning such as static mixer, spinneret, obtained frozen glue precursor will be wrapped by circular blow equipment in it
After the most of good solvent recycling contained, then optimized improved upper cluster tool positioned at path entrance and connects path and go out
The winding apparatus of mouth, precursor obtain high power jet stretch, obtain nascent the having of UHMWPE mixed resin solution dry spinning preparation
Color fibre obtains finished product ultra-high molecular weight polyethylene colored fibers through high power multistage first break draft, samples to finished fiber and carry out spy
Property test, the characteristic index part such as intensity, modulus, fiber number, color fastness is shown in Table 2.
Example 3
It is 5,000,000 UHMWPE resins, 190 liters of decahydronaphthalenes, 2,6 di-t-butyl of antioxidant by the Relative average molecular weight of 14KG
The additive amount of paracresol is respectively 0.5%, 0.7%, the 0.9% of UHMWPE weight resin with this, is uniformly mixed by coppers, note
Enter the solution in special raw material configuration system and twine swelling 3.5 hours in kettle, is injected in homogeneous kettle by reflux delivery pump and further cut
It cuts, sampling at this time carries out the fluid rheology test of the mixed solution, and data result is shown in Table 1, and mixed solution is logical later
Crossing the storage tank with stirring quantitatively to enter shear rate is that the spinning such as 80rpm double screw extruder, static mixer, spinneret are set
Standby extruding spinning, after obtained frozen glue precursor is recycled the most of good solvent for including in it by circular blow equipment, then it is optimized
The improved winding apparatus exported positioned at the upper cluster tool of path entrance and connection path, precursor obtain the drawing of high power spray head
It stretches, obtains the nascent colored fibre of UHMWPE mixed resin solution dry spinning preparation, obtain finished product through high power multistage first break draft
Ultra-high molecular weight polyethylene colored fibers sample finished fiber and carry out characteristic test, intensity, modulus, fiber number, color fastness etc.
Characteristic index part is shown in Table 2.
Example 4
By UHMWPE resin (Relative average molecular weight is 6,000,000), 190 liters of good solvents (preferably decahydronaphthalenes), the antioxygens of 15KG
(Β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester of agent four and phosphorous acid three (2,4- di-tert-butyl-phenyl)
The ratio of ester is 1:1, and additive amount is respectively 0.5%, 0.7%, the 0.9% of UHMWPE weight resin with this, is mixed by coppers equal
Solution even, in injection special raw material configuration system twines swelling 3.5 hours in kettle, is injected in homogeneous kettle by reflux delivery pump into one
Step shearing, at this time sampling carry out the fluid rheology test of the mixed solution, and data result is shown in Table 1, mixes later molten
Liquid passes through the storage tank with stirring and quantitatively enters double screw extruder (shear rate 80rpm), static mixer, spinneret etc.
Spinning equipment extruding spinning, after obtained frozen glue precursor is recycled the most of good solvent for including in it by circular blow equipment, then
The optimized improved winding apparatus exported positioned at the upper cluster tool of path entrance and connection path, precursor obtain high power
Jet stretch obtains the nascent colored fibre of UHMWPE mixed resin solution dry spinning preparation, obtains through high power multistage first break draft
Finished product ultra-high molecular weight polyethylene colored fibers are obtained, finished fiber is sampled and carries out characteristic test, intensity, modulus, fiber number, color
The characteristic index part such as fastness is shown in Table 2.
Example 5
By UHMWPE resin (Relative average molecular weight is 6,000,000), 190 liters of good solvents (preferably decahydronaphthalenes), the antioxygens of 16KG
(Β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester of agent four and phosphorous acid three (2,4- di-tert-butyl-phenyl)
The ratio of ester is 3:1, and additive amount is respectively 0.5%, 0.7%, the 0.9% of UHMWPE weight resin with this, is mixed by coppers equal
Solution even, in injection special raw material configuration system twines swelling 3.5 hours in kettle, is injected in homogeneous kettle by reflux delivery pump into one
Step shearing, at this time sampling carry out the fluid rheology test of the mixed solution, and data result is shown in Table 1, mixes later molten
Liquid passes through the storage tank with stirring and quantitatively enters double screw extruder (shear rate 100rpm), static mixer, spinneret
Equal spinning equipments extruding spinning, after obtained frozen glue precursor is recycled the most of good solvent for including in it by circular blow equipment,
The optimized improved winding apparatus exported positioned at the upper cluster tool of path entrance and connection path, precursor obtain height again
Times jet stretch obtains the nascent colored fibre of UHMWPE mixed resin solution dry spinning preparation, through high power multistage first break draft
Obtain finished product ultra-high molecular weight polyethylene colored fibers, to finished fiber sample carry out characteristic test, intensity, modulus, fiber number,
The characteristic index part such as color fastness is shown in Table 2.
Example 6
By UHMWPE resin (Relative average molecular weight is 6,000,000), 190 liters of good solvents (preferably decahydronaphthalenes), the antioxygens of 16KG
(Β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester of agent four and phosphorous acid three (2,4- di-tert-butyl-phenyl)
The ratio of ester is 1:3, and additive amount is respectively 0.5%, 0.7%, the 0.9% of UHMWPE weight resin with this, is mixed by coppers equal
Solution even, in injection special raw material configuration system twines swelling 3.5 hours in kettle, is injected in homogeneous kettle by reflux delivery pump into one
Step shearing, at this time sampling carry out the fluid rheology test of the mixed solution, and data result is shown in Table 1, mixes later molten
Liquid passes through the storage tank with stirring and quantitatively enters double screw extruder (shear rate 80rpm), static mixer, spinneret etc.
Spinning equipment extruding spinning, after obtained frozen glue precursor is recycled the most of good solvent for including in it by circular blow equipment, then
The optimized improved winding apparatus exported positioned at the upper cluster tool of path entrance and connection path, precursor obtain high power
Jet stretch obtains the nascent colored fibre of UHMWPE mixed resin solution dry spinning preparation, obtains through high power multistage first break draft
Finished product ultra-high molecular weight polyethylene colored fibers are obtained, finished fiber is sampled and carries out characteristic test, intensity, modulus, fiber number, color
The characteristic index part such as fastness is shown in Table 2.
The antioxidant antioxidant effect comparison sheet of 1 different ratio of table
Table 2 --- UHMWPE resin finished product colored fibre embodiment sample property list
Claims (9)
1. a kind of ultra-high molecular weight polyethylene colored fibers, it is characterised in that the colored fibre is by ultra-high molecular weight polyethylene
The mixing for having particular fluid rheological property that resin and spinning good solvent, auxiliary agent and inorganic pigment or organic pigment are formed
Solution, the ultra-high molecular weight polyethylene colored fibers prepared by dry spinning processes, intensity are 10 ~ 42g/d, and modulus is
300~1700g/d；The auxiliary agent includes antioxidant.
2. the preparation method of ultra-high molecular weight polyethylene colored fibers according to claim 1, it is characterised in that: the addition
Antioxidant are as follows: four (β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol esters (below with letter four (Β-(3,
5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester reference)；Phosphorous acid three (2,4- di-tert-butyl-phenyl) ester； 2,6
One or more of di-tert-butyl p-cresol.
3. the preparation method of ultra-high molecular weight polyethylene colored fibers according to claim 2, it is characterised in that described is anti-
(Β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester of oxygen agent four or (the 2,4- di-tert-butyl of phosphorous acid three
Base) ester additive amount be 0.1 ~ 2.0%wt.
4. the preparation method of 2 ultra-high molecular weight polyethylene colored fibers according to claim 2, it is characterised in that: described
(Β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester of antioxidant four or (the 2,4- di-tert-butyl of phosphorous acid three
Base) ester additive amount be 0.5 ~ 1.2%wt.
5. the preparation method of ultra-high molecular weight polyethylene colored fibers according to claim 2, it is characterised in that: described is anti-
Oxygen agent is 2,6 di-tert-butyl p-cresol.
6. the preparation method of ultra-high molecular weight polyethylene colored fibers according to claim 2, it is characterised in that: described is anti-
2,6 di-tert-butyl p-cresol additive amount of oxygen agent is 0.2 ~ 1.5%wt.
7. the preparation method of ultra-high molecular weight polyethylene colored fibers according to claim 2, it is characterised in that: described is anti-
2,6 di-tert-butyl p-cresol additive amount of oxygen agent is 0.7 ~ 1.0%wt.
8. the preparation method of ultra-high molecular weight polyethylene colored fibers according to claim 2, it is characterised in that: the antioxygen
(Β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester of agent four and phosphorous acid three (2,4- di-tert-butyl-phenyl)
The compound addition range of ester is 0.3 ~ 1.2%wt；Four (Β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol esters with
Ratio range 5:1 ~ the 1:5 of phosphorous acid three (2,4- di-tert-butyl-phenyl) ester.
9. the preparation method of ultra-high molecular weight polyethylene colored fibers according to claim 2, it is characterised in that: the antioxygen
(Β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester of agent four and phosphorous acid three (2,4- di-tert-butyl-phenyl)
The compound addition range of ester be 0.5 ~ 0.9%wt, four (Β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol esters with
Ratio range 3:1 ~ the 1:3 of phosphorous acid three (2,4- di-tert-butyl-phenyl) ester.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102050980A (en) * | 2009-10-28 | 2011-05-11 | 中国石油化工股份有限公司 | Ultra-high molecular weight polyethylene resin composition |
| CN103866416A (en) * | 2014-03-20 | 2014-06-18 | 剑乔科技江苏有限公司 | Preparation method for ultra-high molecular weight polyethylene colored fibers |
| US20160158976A1 (en) * | 2014-12-03 | 2016-06-09 | Dirk Pletcher | Antioxidant-infused ultra high molecular weight polyethylene |
| CN106544746A (en) * | 2015-09-18 | 2017-03-29 | 中国石油化工股份有限公司 | Ultra-high molecular weight polyethylene mixed solution dry spinning prepares the method and fiber of colored fibre |
-
2017
- 2017-10-19 CN CN201710974022.1A patent/CN109680351A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102050980A (en) * | 2009-10-28 | 2011-05-11 | 中国石油化工股份有限公司 | Ultra-high molecular weight polyethylene resin composition |
| CN103866416A (en) * | 2014-03-20 | 2014-06-18 | 剑乔科技江苏有限公司 | Preparation method for ultra-high molecular weight polyethylene colored fibers |
| US20160158976A1 (en) * | 2014-12-03 | 2016-06-09 | Dirk Pletcher | Antioxidant-infused ultra high molecular weight polyethylene |
| CN106544746A (en) * | 2015-09-18 | 2017-03-29 | 中国石油化工股份有限公司 | Ultra-high molecular weight polyethylene mixed solution dry spinning prepares the method and fiber of colored fibre |
Non-Patent Citations (1)
| Title |
|---|
| 周大纲等编著: "《塑料老化与防老化技术》", 30 November 1998, 中国轻工业出版社 * |
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Application publication date: 20190426 |