CN108004605A - Strong porous superhigh molecular weight polyethylene fibers and preparation method in one kind - Google Patents
Strong porous superhigh molecular weight polyethylene fibers and preparation method in one kind Download PDFInfo
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- CN108004605A CN108004605A CN201711427203.9A CN201711427203A CN108004605A CN 108004605 A CN108004605 A CN 108004605A CN 201711427203 A CN201711427203 A CN 201711427203A CN 108004605 A CN108004605 A CN 108004605A
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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
- D01D5/12—Stretch-spinning methods
-
- 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
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- 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
- D01D10/06—Washing or drying
-
- 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
- D01D5/06—Wet spinning methods
-
- 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
-
- 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
Abstract
The invention discloses strong porous superhigh molecular weight polyethylene fibers and preparation method in one kind, the fiber is ultra-high molecular weight polyethylene as raw material, UHMWPE frozen glue precursor is prepared by gel spinning method, is stretched using level-one, prepared by fixed length extraction and dry, secondary drawing technique.UHMWPE fiber functionalization can be achieved, its product has the characteristics that high porosity, moderate strength, impact resistance, wear-resisting, corrosion-resistant, it can be used as sorbing material or the composite material of moderate strength uses, such as extraction of uranium from seawater, administer amber pollution, building industry.
Description
Technical field
The invention belongs to chemical fiber field, and in particular in a kind of strong porous superhigh molecular weight polyethylene fibers and
Preparation method.
Background technology
Ultra-high molecular weight polyethylene（UHMWPE）Fiber is also known as high-strength high-modulus polyethylene（PE）Fiber, by averagemolecular wt
Measure the spinnings of the PE more than 1,000,000 to form, be another high intensity, the high-modulus occurred after carbon fiber and aramid fiber
High-performance fiber, UHMWPE have identical molecular structure with common PE, and main chain chain link is（-CH2-CH2-）, but it is high
Molecular weight assigns many common PE fibers of UHMWPE fibers incomparable excellent properties.In addition to intensity height, it also has
Performance, its shock resistance such as excellent impact resistance, resistant to chemical etching and self-lubricating are highest in all high molecule plastics, and
It can work for a long time under the conditions of -160 DEG C ~+80 DEG C, be referred to as the engineering plastics of " surprising ".Because of its excellent performance,
UHMWPE fibers have been widely used for weaving, chemical industry, food, agricultural, building, medical treatment, physical culture, military and national defense and aerospace etc.
Field, such as protective materials, high-strength rope, composite material, movable machinery and flak jackets etc..
With the development that the epoch are at full speed, the serious energy crisis of facing mankind and problem of environmental pollution.It is many in terms of the energy
More researchers start to tap a new source of energy so that instead of traditional energy, such as the extraction of uranium from seawater etc., China starts to grind in the 1970s
Study carefully the extraction of uranium from seawater, research finds that the key technology of the extraction of uranium from seawater is to obtain suitable adsorbent, adsorbent need to meet capacity it is big,
The features such as efficient, selective good, chemical stabilization, good, corrosion-resistant, pollution-free mechanical strength, if original in UHMWPE fibers
Increase the loose structure of high specific surface area on the basis of characteristic or by grafted propylene acid, acrylonitrile on the hydrocarbon backbone of PE
Deng group, acid amides analog copolymer is generated, then the Selective adsorption function of UHMWPE fibers can be achieved.
On the other hand, the heavy metal pollution in seawater, lake and the eutrophication problem because of elements such as nitrogen, phosphorus, also may be used
Solved by the high adsorption material with loose structure.This porous material can not only adsorb, filtering oil, heavy metal and
Trace element, also to possess higher intensity, wear-resisting, shock resistance and it is corrosion-resistant the features such as.Due to UHMWPE fibrous material density
It is smaller than water, it can bubble through the water column and there is high intensity, corrosion-resistant, impact resistance.So the UHMWPE fibers of loose structure will
It is one of optimal material as water surface absorption.
The content of the invention
Present invention generally provides strong porous superhigh molecular weight polyethylene fibers and preparation method in one kind, it is made of the fiber
Textile, be applicable to filtering material and can also be applied to the fields such as the civil and military of moderate strength composite material.
The above-mentioned technical problem of the present invention mainly solves by the following technical programs：Strong porous super high molecular weight is gathered in one kind
Vinyl fiber, is to be positioned over UHMWPE powder in white oil solvent, the M in UHMWPE powderwGenerally greater than 1 × 106More than, add
Enter appropriate antioxidant, emulsifying agent, aluminum stearate and stir evenly and prepare spinning solution, then gather cold formed after spinneret is extruded and freeze
Collagen silk.Then by frozen glue precursor level-one drawing by high temperature, then fixed length extraction and dry obtained UHMWPE protofibres, protofibre
Strong porous superhigh molecular weight polyethylene fibers in being made described through two level drawing by high temperature again.
Preferential be：It is 65 ~ 75mPa.s at 40 DEG C of the kinematic viscosity of the dissolvant white oil.
Preferential be：The mass percentage concentration that emulsifying agent accounts for ultra-high molecular weight polyethylene is 0.003 ~ 0.0035%, antioxygen
The mass percentage concentration that agent accounts for ultra-high molecular weight polyethylene is 0.2 ~ 0.5%.
Preferential be：The first spinning frozen glue precursor is hypocrystalline state, the amorphous being made of the strand crimped
The crystalline region composition that the strand of area and regular folding is formed.Can be orientated fiber molecule chain after level-one drawing by high temperature.
Preferential be：Fixed length extracts and drying, fiber produce substantial amounts of pore space structure after agent for carbon hydrogen detergent extracts.
The present invention also provides the preparation process of strong porous superhigh molecular weight polyethylene fibers in a kind of, its manufacture craft press with
Lower step：
1) spinning solution is prepared
Quantitative white oil is heated to 50 ~ 60 DEG C, is by weight white oil under stirring：Ultra-high molecular weight polyethylene is 10:
1 ratio, adds ultra-high molecular weight polyethylene powder, adds emulsifying agent, aluminum stearate, antioxidant and opens mulser and make superelevation
Molecular weight polyethylene is sufficiently mixed with white oil, by obtained mixed material be transferred to swelling kettle and carry out heating stirring 2 ~ 4 it is small when,
Temperature is 90 ~ 120 DEG C.
2) superhigh molecular weight polyethylene fibers gel fiber is prepared
Spinning solution after swelling is transported in twin (double) screw extruder, by twin-screw extruder, melt, be stirred it is super
High molecular weight polyethylene strand fully solution in the state of white oil dissolving is penetrated into twines, and wherein extruder temperature control is 250 ~ 300
Between DEG C, then through filament spinning component spinneret, the filament of viscous state frozen glue precursor is formed after circulating water.
3) frozen glue precursor balances
Frozen glue precursor is placed under room temperature environment, when balance 24 ~ 48 is small, ensures temperature at 22 ~ 30 DEG C, humidity is 65 ± 5%, and
Frozen glue precursor is shunk to the white oil gone out to exclude.
4) level-one drawing by high temperature frozen glue precursor
By the frozen glue precursor after balance using draw ratio as 7 ~ 11 boiling water bath cabinets for passing through 90 ~ 100 DEG C after creel.This was stretched
For journey since frozen glue precursor contains substantial amounts of white oil, fibrous inside solvent lubricating effect is notable, the main sliding that strand occurs and
The orientation of strand, is changed from chain-folded lamellae to extended-chain lamellae.
5) fixed length extraction and drying
Frozen glue precursor after level-one drawing by high temperature is extracted in the ultrasonic extraction groove containing hydrocarbon extractant, and in negative pressure
Drawing-off is dried in 35 ~ 50 DEG C of drying box, draw ratio 1:01~1:20, strong porous fibre spun filament in being prepared into.
6) two level high drafting
Strong porous superhigh molecular weight polyethylene fibers spun filament two level drawing-off in 105 ~ 120 DEG C of hot tank, draw ratio 4 by
~ 5, strong porous superhigh molecular weight polyethylene fibers in being then made after rolled machine winding.
Step（1）In, the average molar mass of the ultra-high molecular weight polyethylene powder is 100 ~ 6,000,000, described
The mass concentration of aluminum stearate is the 0.001 ~ 0.005% of ultra-high molecular weight polyethylene, and the mass concentration of the antioxidant is super
The 0.1 ~ 0.5% of High molecular weight polyethylene, the mass concentration of the emulsifying agent for ultra-high molecular weight polyethylene 0.003 ~
0.001%, mixing speed is 60 ~ 80r/min in the swelling kettle.
Step（4）In, level-one drawing by high temperature frozen glue precursor, frozen glue precursor is impregnated in drawing-off in boiling water bath, this was stretched
Fibrous inside solvent lubricating effect is notable in journey, the orientation effect of the main sliding and strand that strand occurs, strand by
Chain-folded lamellae changes to extended-chain lamellae.
Step（5）In, frozen glue precursor fixed length extraction and drying under ul-trasonic irradiation after drawing-off, strand is radially receipts
Contracting, draw ratio 1:01~1:20, fiber porosity increase.
Step（6）In, the two level super drawing, tensile strain rate 1S-1, make the macromolecular orientation in fiber,
Chain-folded lamellae changes to extended chain is brilliant, and fibre strength and modulus increase sharply.
Beneficial effects of the present invention：Fibrous inside is macromolecular entangled to each other after gel spinning and extraction drying process
Network structure, and a large amount of gaps are left in the position of solvent volatilization, non-stretched preceding due to short texture, fiber mechanical strength is very
Low, no actual use value, so post-tensioning need to be carried out to fiber, makes macromolecular chain orientation arrive extended chain again to chain-folded lamellae
Brilliant transformation, during this high power hot-stretch, since the regular precise alignment of fiber molecule chain makes fibre strength and mould
Amount is increased dramatically, but also greatly reduces loose structure therein.
Embodiment
With reference to embodiment, the present invention is described in detail, and following embodiments are explanation of the invention and of the invention
It is not limited to following embodiments.
The present embodiment provides strong porous superhigh molecular weight polyethylene fibers, the fiber in one kind to be placed with UHMWPE powder
In white oil solvent, add appropriate antioxidant, emulsifying agent, aluminum stearate and stir evenly and prepare spinning solution, then through spinneret
Gather cold formation frozen glue precursor after extrusion；Then by frozen glue precursor level-one drawing by high temperature, then fixed length extraction and dry obtained UHMWPE
Protofibre, protofibre strong porous superhigh molecular weight polyethylene fibers in being made described through two level drawing by high temperature again.
The frozen glue precursor that just spins is hypocrystalline state, the amorphous area being made of the strand crimped and regular folding
The crystalline region composition that strand is formed；Can be orientated fiber molecule chain after level-one drawing by high temperature.The fixed length is extracted and done
Dry, fiber produces substantial amounts of pore space structure after agent for carbon hydrogen detergent extracts.
The present embodiment also provide it is a kind of in strong porous superhigh molecular weight polyethylene fibers preparation method, the preparation method
Carry out according to the following steps：
1) spinning solution is prepared
Quantitative white oil is heated to 55 DEG C, is by weight white oil under stirring：Ultra-high molecular weight polyethylene is 10:1
Ratio, adds ultra-high molecular weight polyethylene powder, adds emulsifying agent, aluminum stearate, antioxidant and opening mulser divides superelevation
Sub- weight northylen is sufficiently mixed with white oil, by obtained mixed material be transferred to swelling kettle and carry out heating stirring 3 it is small when, temperature
For 100 DEG C.
2) superhigh molecular weight polyethylene fibers gel fiber is prepared
Spinning solution after swelling is transported in twin (double) screw extruder, by twin-screw extruder, melt, be stirred it is super
High molecular weight polyethylene strand white oil dissolving penetrate into the state of fully solution twine, wherein extruder temperature control 280 DEG C it
Between, then through filament spinning component spinneret, the filament of viscous state frozen glue precursor is formed after 23 DEG C of circulating water.
3) frozen glue precursor balances
Frozen glue precursor is placed on temperature as 24 DEG C, when balance 30 is small in the environment of humidity is 65%, and frozen glue precursor is shunk what is
White oil excludes.
4) level-one drawing by high temperature frozen glue precursor
Frozen glue precursor after balance is passed through into 90 DEG C of circulating boiling water bath after creel with 8 draw ratio, and by boiling water bath
The white oil squeezed out due to drawing of fiber and water separation recycling in groove.
5) fixed length extraction and drying
Frozen glue precursor after level-one drawing by high temperature is extracted in the ultrasonic extraction groove containing hydrocarbon extractant, solvent and extraction
The double diffusion effect of agent makes strand crystalline region and amorphous area diffuse into one another interference, is led after extraction in the drying box that negative pressure is 40 DEG C
Stretch drying, the volatilization of extractant causes in fiber between strand in drying process and strand itself produces tensile force, makes point
The different degrees of contraction of subchain.Strong porous fibre spun filament in being prepared into after extractant volatilization.
6) two level high drafting
Strong porous superhigh molecular weight polyethylene fibers spun filament two level drawing-off in 110 DEG C of hot tank by, draw ratio are 4 ~ 5,
Then strong porous superhigh molecular weight polyethylene fibers in being made after rolled machine winding.
Detect data：
| Fiber dimensious（dtex） | Fracture strength（CN/dtex） | Elongation at break（%） | Rupture modulus（CN/dtex） | Porosity |
| 400 | 12~16 | 1~2.2 | 500~1100 | 45.5% |
Claims (10)
1. strong porous superhigh molecular weight polyethylene fibers in one kind, it is characterised in that：The fiber is positioned over UHMWPE powder
In white oil solvent, add appropriate antioxidant, emulsifying agent, aluminum stearate and stir evenly and prepare spinning solution, then squeezed through spinneret
Gather cold formation frozen glue precursor after going out；Then by frozen glue precursor level-one drawing by high temperature, then fixed length extraction and dry obtained UHMWPE originals
Raw fiber, protofibre strong porous superhigh molecular weight polyethylene fibers in being made described through two level drawing by high temperature again.
2. strong porous superhigh molecular weight polyethylene fibers in one kind as claimed in claim 1, it is characterised in that：The solvent is white
It is 65 ~ 75mPa.s at 40 DEG C of the kinematic viscosity of oil.
3. strong porous superhigh molecular weight polyethylene fibers in one kind as claimed in claim 1, it is characterised in that：The emulsifying agent
The mass percentage concentration for accounting for ultra-high molecular weight polyethylene is 0.003 ~ 0.0035%, and antioxidant accounts for the matter of ultra-high molecular weight polyethylene
It is 0.2 ~ 0.5% to measure percentage concentration.
4. strong porous superhigh molecular weight polyethylene fibers in one kind as claimed in claim 1, it is characterised in that：Described just spin is frozen
Collagen silk is hypocrystalline state, the crystalline region group that the strand of the amorphous area being made of the strand crimped and regular folding is formed
Into can be orientated fiber molecule chain after level-one drawing by high temperature.
5. strong porous superhigh molecular weight polyethylene fibers in one kind as claimed in claim 1, it is characterised in that：The fixed length extraction
Take and dry, fiber produces substantial amounts of pore space structure after agent for carbon hydrogen detergent extracts.
6. it is a kind of as described in claim 1-5 in strong porous superhigh molecular weight polyethylene fibers preparation method, its feature exists
In：The preparation method carries out according to the following steps：
Prepare spinning solution
Quantitative white oil is heated to 50 ~ 60 DEG C, the addition ultra-high molecular weight polyethylene powder under stirring, addition emulsifying agent,
Aluminum stearate, antioxidant and opening mulser is sufficiently mixed ultra-high molecular weight polyethylene and white oil, the mixed material that will be obtained
Be transferred to swelling kettle and carry out heating stirring 2 ~ 4 it is small when, temperature be 90 ~ 120 DEG C；
Prepare superhigh molecular weight polyethylene fibers gel fiber
Spinning solution after swelling is transported in twin (double) screw extruder, by twin-screw extruder, melt, be stirred it is super
High molecular weight polyethylene strand fully solution in the state of white oil dissolving is penetrated into twines, and wherein extruder temperature control is 250 ~ 300
Between DEG C, then through filament spinning component spinneret, the filament of viscous state frozen glue precursor is formed after 22 ~ 25 DEG C of circulating water；
Frozen glue precursor balances
By frozen glue precursor be placed under room temperature environment balance 24 ~ 48 it is small when, and frozen glue precursor is shunk to the white oil gone out and is excluded；
Level-one drawing by high temperature frozen glue precursor
Frozen glue precursor after balance is passed through into 80 ~ 100 DEG C of circulating boiling water bath after creel with 7 ~ 11 draw ratio, and will
The white oil squeezed out due to drawing of fiber and water separation recycling in boiling water bath；
Fixed length extracts and drying
Frozen glue precursor after level-one drawing by high temperature is extracted in the ultrasonic extraction groove containing hydrocarbon extractant, solvent and extraction
The double diffusion effect of agent makes strand crystalline region and amorphous area diffuse into one another interference, in the drying box that negative pressure is 35 ~ 50 DEG C after extraction
Middle drawing-off drying, the volatilization of extractant causes in fiber between strand in drying process and strand itself produces tensile force,
Make the contraction that strand is different degrees of；
Strong porous fibre spun filament in being prepared into after extractant volatilization；
Two level high drafting
Strong porous superhigh molecular weight polyethylene fibers spun filament two level drawing-off in 105 ~ 140 DEG C of hot tank, draw ratio 4 by
~ 5, strong porous superhigh molecular weight polyethylene fibers in being then made after rolled machine winding.
7. it is according to claim 6 it is a kind of in strong porous superhigh molecular weight polyethylene fibers preparation method, its feature exists
In：Step（1）In, the average molar mass of the ultra-high molecular weight polyethylene powder is 100 ~ 6,000,000, the stearic acid
The mass concentration of aluminium is the 0.001 ~ 0.005% of ultra-high molecular weight polyethylene, and the mass concentration of the antioxidant is supra polymer
The 0.1 ~ 0.5% of weight northylen, the mass concentration of the emulsifying agent are the 0.003 ~ 0.001% of ultra-high molecular weight polyethylene, institute
Mixing speed is 60 ~ 80r/min in the swelling kettle stated.
8. it is according to claim 6 it is a kind of in strong porous superhigh molecular weight polyethylene fibers preparation method, its feature exists
In：Step（4）In, level-one drawing by high temperature frozen glue precursor, frozen glue precursor is impregnated in drawing-off in boiling water bath, fine in this drawing process
Dimension internal solvent lubricating effect is notable, and the orientation effect of the main sliding and strand that strand occurs, strand is by folded chain
Piece crystal orientation extended-chain lamellae changes.
9. it is according to claim 1 it is a kind of in strong porous superhigh molecular weight polyethylene fibers preparation method, its feature exists
In：Step（5）In, frozen glue precursor fixed length extraction and drying under ul-trasonic irradiation after drawing-off, strand is radial contraction, is led
Stretch than for 1:01~1:20, fiber porosity increase.
10. it is according to claim 1 it is a kind of in strong porous superhigh molecular weight polyethylene fibers preparation method, its feature exists
In：Step（6）In, the two level super drawing, tensile strain rate 1S-1, make the macromolecular orientation in fiber, folded chain
The brilliant transformation of piece crystal orientation extended chain, fibre strength and modulus increase sharply.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109440220A (en) * | 2018-09-11 | 2019-03-08 | 江苏恒辉安防股份有限公司 | Cut resistant fibers and preparation method thereof |
| CN109468689A (en) * | 2018-12-06 | 2019-03-15 | 长青藤高性能纤维材料有限公司 | A kind of ultra high molecular weight polyethylene fiber gel spinning method and the soft kneading machine of double ranks using the soft kneading machine of double ranks |
| CN110318116A (en) * | 2019-05-29 | 2019-10-11 | 长青藤高性能纤维材料有限公司 | A kind of preparation method of extra-high strong ultra high molecular weight polyethylene fiber |
| CN110438582A (en) * | 2019-07-30 | 2019-11-12 | 青岛信泰科技有限公司 | A kind of preparation method of oil suction ultra high molecular weight polyethylene fiber |
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| CN110438582B (en) * | 2019-07-30 | 2022-03-01 | 青岛信泰科技有限公司 | Preparation method of oil-absorbing ultra-high molecular weight polyethylene fiber |
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