CN108950714A - A kind of superelevation is strong, Gao Mo, fine count fiber preparation method - Google Patents
A kind of superelevation is strong, Gao Mo, fine count fiber preparation method Download PDFInfo
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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
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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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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Abstract
Strong, Gao Mo, fine count fiber preparation method that the present invention relates to a kind of superelevation.Its preparation step are as follows: polyvinyl resin with super-high molecular weight powder and solvent A are subjected to first time physical mixed；The extra solvent A for being attached to polyvinyl resin with super-high molecular weight powder surface is removed through sieving, centrifugation；Second of physical mixed is carried out with solvent B and additive；Mixed slurry injects double screw extruder, is squeezed out by metering pump, filament spinning component and spinneret；Gel fiber carries out preliminary draft at room temperature, and is extracted and dried；Dry silk is cooled to room temperature winding and obtains finished silk through multistage hot gas spring.The present invention prepares that the superelevation that has excellent performance is strong, Gao Mo, fine count fiber under optimal conditions.The present invention can be used for manufacturing the high value added products such as high-performance laminated cloth, flak jackets, bulletproof halmet, bulletproof armour plate, anti-cutting gloves.
Description
Technical field
The invention belongs to polymeric material fields, and in particular to a kind of superelevation is strong, Gao Mo, fine count fiber preparation method.
Background technique
Fiber typically refers to the anisotropic material that length is much larger than width and thickness, with mentioning for anisotropic degree
Height, physical properties in the longitudinal direction gradually increase, while remain excellent flexibility and machinability.Fiber
It is many kinds of, wherein high-performance fiber becomes what various countries competitively researched and developed since performance is prominent, added value is high, technical difficulty is big
Emphasis.By taking ultra-high molecular weight polyethylene (UHMWPE) fiber as an example, external to realize industrialization the eighties in last century, China is with peaceful
Key technology is broken through the nineties in last century headed by wave great achievement and large-scale production is carried out based on independent intellectual property right.Currently, quotient
The highest nominal strength of product UHMWPE fiber is 42.5cN/dtex (about 4.1GPa), and the theory of UHMWPE fiber is most high-strength
Degree is it is generally acknowledged that up to 10~20GPa.As it can be seen that the room for promotion of fibre property is still very big.
Gel spinning is the UHMWPE fiber production method generallyd use both at home and abroad, has lot of documents report and patent is protected
Shield, for example, document [Makromol.Chem., 1979,189:2983-2986；J.Mater.Sci., 1980,15:505-514；
J.Polym.Sci.Pt.B-Polym.Phys., 1994,32:261-269] and patent of invention [NL19790004990；
US4413110；US5578374；JP58167170；CN1268588；CN101724921A；CN102002769A], etc..Frozen glue
Spining technology is big for UHMWPE resin viscosity, is difficult to the problems such as melt-processed, first by UHMWPE resin dispersion in good solvent
In, solution and gel fiber are formed by modes such as twin-screw extrusions, then removes solvent, and carries out super times hot gas spring, is prepared
High-strength, high mould UHMWPE fiber.Although the prior art can smoothly produce UHMWPE fiber, mass production practice and experiment are ground
Study carefully and also discloses many urgent problems to be solved.Especially the initial feed of gel spinning is UHMWPE toner and small molecule
The nature difference of solvent, the two is very big, be easy to happen in mixing, transmission and course of dissolution toner aggregation, adherency and
Sedimentation is unfavorable for draft ratio and improves and preparation to cause the problems such as concentration of dope is uneven, difference is big between fiber strand silk
The uniform fine count fiber of structure, this has become one of the major technology bottleneck of constraints on fiber performance improvement and quality-improving.
Summary of the invention
Present invention status in view of the above technology, provides that a kind of superelevation is strong, preparation method of Gao Mo, fine count fiber.
The present invention is directed to the physics of polyvinyl resin with super-high molecular weight powder and spin solvent in conventional gel spinning technology
Nature difference is big, such as the density and viscosity of polyvinyl resin with super-high molecular weight powder are greater than spin solvent, to cause spinning
The problems such as solution is uneven, difference is big between fiber strand silk, is tightly thought deeply and many experiments, proposes strong a kind of superelevation, Gao Mo, thin
The preparation method of denier fiber.
The method of the present invention the following steps are included:
Ultra-high molecular weight polyethylene (UHMWPE) toner and relative density at room temperature are lower than 0.75g/ by step (1)
cm3And solvent A of the boiling point higher than 100 DEG C carries out first time physical mixed under normal pressure；
Wherein the weight ratio of polyvinyl resin with super-high molecular weight powder and solvent A is 51/49~99/1；Preferably,
The weight ratio of polyvinyl resin with super-high molecular weight powder and solvent A is 75/25~99/1；
The weight average molecular weight of the polyvinyl resin with super-high molecular weight powder is 3,000,000~6,000,000, and molecular weight distribution is
2.0~4.0, the side chain number of every 10000 carbon atoms is 0.1~1；
Preferably, the average grain diameter of the polyvinyl resin with super-high molecular weight powder is 10~90 microns, partial size point
Cloth is 1.5~3.5, and average crystallinity is 55%~75%；Further preferably, the polyvinyl resin with super-high molecular weight powder
Average grain diameter be 10~50 microns, particle diameter distribution be 1.5~2.5；
The solvent A is the one or more mixtures for the alkane that carbon atom number is 7~12；
The first time physical mixed in the closed container with agitating device and pressure and temperature control into
Row, stirring rate are 100~900rpm, and pressure is 1.2~2.8 atmospheric pressure, and temperature is 20~100 DEG C, incorporation time 10
~90 minutes；
The mixture that step (2) obtains step (1) stands, balances to room temperature, then removes through sieving, centrifugation
It is attached to the extra solvent A on polyvinyl resin with super-high molecular weight powder surface, mesh number is used to carry out for 180~240 sieve
Sieving, weight content of the final solvent A in toner are 0.1%~4.9%；
Preferably, final weight content of the solvent A in polyvinyl resin with super-high molecular weight powder be 0.1%~
2.5%；
The mixture and solvent B and additive that step (3) obtains step (2) carry out second of physical mixed, are mixed into
Mixed slurry；
The weight ratio of mixture and solvent B that wherein step (2) obtains is 8/92~16/84, additive level≤
5wt%；
The solvent B is one of paraffin oil, mineral oil, kerosene or mixture that is any number of and arbitrarily matching；
The additive includes antioxidant, lubricant, antistatic agent, the ultra-violet stabilizer of any proportion；
Second of physical mixed is carried out in closed have in agitating device and temperature controlled container, is stirred
Rate is 10~60rpm, and temperature is 20~100 DEG C, and incorporation time is 10~30 minutes；
The mixed slurry that step (4) obtains step (3) injects double screw extruder, by metering pump, filament spinning component and
Spinneret squeezes out, and enters in circulating cooling water-bath through the air gap, and gel fiber, which is orderly fallen into, under the traction of drive roll contains silk cylinder；
The screw diameter of the double screw extruder be 65~95mm, draw ratio be 60~80, barrel temperature be 180~
260 DEG C, screw speed is 150~350rpm；
The temperature of the filament spinning component and spinneret is 240~260 DEG C；
The spinneret is round spinneret, and hole count is 240~480, and aperture is 0.6~1.0mm, draw ratio is 8~
12；
The air gap length is 2~10mm, and cooling bath temperature is 5~25 DEG C, and the draw-down rate of drive roll is 5
~25m/min；
Preferably, the air gap length is 2~6mm, and applies drawing-off, drawing-off to strand in the air gap
It is 4~6 than DR1；
The gel fiber that step (4) obtains is stood 16~48 hours by step (5) at room temperature, is then carried out at room temperature
Preliminary draft, and continuity enter extraction tank and drying box and extracted and dried；
The preliminary draft ratio DR2 is 8~12；
Extractant in the extraction tank is one of agent for carbon hydrogen detergent, gasoline, methylene chloride, carbon tetrachloride or appoints
Meaning kind and the mixture arbitrarily matched；
Preferably, carrying out drawing-off to strand in extraction, drying process, draw ratio DR3 is 1.2~1.6:
The drying silk that step (6) obtains step (5) imports steam hot tank through seven roller drafting machines and carries out multistage hot gas spring,
Then drafting silk is cooled to room temperature in the case where keeping tension state, winding obtains finished silk；
Preferably, 1~3 traction roller of the seven roller drafting machines in neighbouring hot tank side is hot-rolling, roll surface temperature
It spends consistent with the temperature of hot tank inlet；
Preferably, the multistage hot gas spring is three-level hot gas spring, draw ratio DR4 is 6~9.
The excellent effect of the present invention is that:
Method of the invention has surprisingly obtained high uniformity, stable spinning solution and multifibres strand, to have
Effect solve the above problem existing for conventional gel spinning technology, produce breaking strength >=39cN/dtex, initial modulus >=
1250cN/dtex, filament number≤1.50dtex, irregularity≤3.5% high-performance UHMWPE fiber.
The novelty and creativeness of the method for the present invention are embodied in many aspects.Firstly, by polyvinyl resin with super-high molecular weight
Powder and solvent A carry out first time physical mixed, obtain modified mixture, and wherein solvent A is that density is lower, boiling point is higher small
Molecule alkane, scattering and permeating enters UHMWPE toner in mixed process, thus reduce the density of UHMWPE toner,
Its specific surface area and surface layer porosity are improved, is conducive to subsequent and solvent B and prepares homogeneous solution progress gel spinning.By a large amount of
It tests repeatedly, the special properties and mixing condition of discovery polyvinyl resin with super-high molecular weight powder and solvent A are for described
Scattering and permeating process and its effect are most important.For example, when the average grain diameter of toner is excessive, one side scattering and permeating institute
The overlong time needed, the solvent A content on the other hand eventually entering into polyvinyl resin with super-high molecular weight powder is very few, thus up to not
Still there is polyvinyl resin with super-high molecular weight powder in subsequent formulation solution in the degree reduced to required toner density
The problem of end settles in the lower solvent B of density；And when the average grain diameter of polyvinyl resin with super-high molecular weight powder is too small,
Since specific surface area is excessive, the problems such as frequently occurring aggregation during the preparation process, adhere to, equally it is unfavorable for the reality of the object of the invention
It is existing.On the other hand, it finds in many experiments, using modification mixture of the invention as gel spinning raw material, not only prepares
Dissolved efficiency when solution significantly improves, it is no longer necessary to which routine techniques is with high temperature, high shear and for a long time for the molten of main feature
Solution preocess, to substantially alleviate polyvinyl resin with super-high molecular weight in dissolution, the degradation in spinning process, and strand is led
Stretching property significantly improves, and total stretch ratio is up to 400~600 in optimal conditions, far more than conventional gel spinning technology at other
Total stretch ratio (≤300) when part is identical.In the first time physical mixed stage of the invention under the optimal conditions scattering and permeating
Appropriate solvent A into UHMWPE toner plays irreplaceable role, it is likely that promotes superhigh molecular weight polyethylene
The strand disentanglement of olefine resin.It is well known that for gel spinning technology, in order to improve the drawability of strand in turn
Improve the performance of finished silk, one of most important precondition is exactly the UHMWPE resin for selecting entanglement degree low as far as possible.
The present invention is exactly based on the polyvinyl resin with super-high molecular weight powder progress physical mixed to specific structure property and changes
Property, this important prerequisite is met under optimal conditions, to prepare, the superelevation that has excellent performance is strong, Gao Mo, fine count fiber.
The present invention can be used for manufacturing high-performance laminated cloth, flak jackets, bulletproof halmet, bulletproof armour plate, anti-cutting gloves etc.
High value added product.
Specific embodiment
Technical solution of the present invention and effect are further described below with reference to embodiment.Supra polymer in embodiment
The weight average molecular weight and molecular weight distribution of weight ethylene resin powder use the High Temperature Gel Permeation color of model PL-GPC 220
Spectrometer measurement；Average crystallinity is measured using the polycrystal X ray diffractometer of model D8 Advance Davinci；Average grain diameter
It is measured with particle diameter distribution using the laser particle size analyzer of model S3500；Solvent A is in polyvinyl resin with super-high molecular weight powder
In amount retained using extraction, weight method measurement.
Embodiment 1:
Take 99 kilograms of polyvinyl resin with super-high molecular weight powder with 1 kilogram of alkane solvent in closed double-jacket conduction oil
First time physical mixed is carried out in the high-speed mixer of heating；Wherein, the Weight-average molecular of polyvinyl resin with super-high molecular weight powder
Amount is 3,000,000, the side chain number of molecular weight distribution 2.0, every 10000 carbon atoms is 0.1, average grain diameter is 10 micron,
Diameter is distributed as 1.5, average crystallinity 55%；Alkane solvent is mixed by heptane and octane with volume ratio 40/60, in room
Relative density under temperature is 0.69, the boiling point under normal pressure is 120 DEG C；Stirring rate in high-speed mixer is 100rpm, pressure
For 1.2 atmospheric pressure, temperature is 20 DEG C；Mixing stops stirring after ten minutes, and mixture is taken out in release, stands, balances to room temperature,
Sieving, centrifugation are carried out using the sieve of 240 mesh, obtain the mixture that alkane solvent content is about 0.1wt%；Take this mixture 16
Kilogram second of physical mixed is carried out in closed stirred tank with 84 kilograms of kerosene and 1 kilogram of antioxidant, in stirred tank
Stirring rate is 60rpm, and temperature is 60 DEG C；After ten minutes, by slurry injection screw diameter be 65mm, draw ratio is 80 for mixing
Double screw extruder, barrel temperature are 180~240 DEG C, screw speed 350rpm；Being delivered to temperature through metering pump is 240 DEG C
Filament spinning component and hole count is 480, aperture 1.0mm, draw ratio are 8 spinneret；Extrusion solution is by between the air of 2mm
Gap, the cooling bath for being 25 DEG C into temperature, gel fiber, which draws to fall into the rate of 25m/min through drive roll, contains silk cylinder, in sky
Drawing-off is applied to strand in gas gap；Gel fiber stands 16 hours at room temperature, then carries out preliminary draft at room temperature, and continuous
Property enter the extraction tank containing agent for carbon hydrogen detergent and air dry oven and extracted and dried, measure the Weight-average molecular of dry silk
Amount is 2,680,000, carries out drawing-off to strand in extraction, drying process；Dry silk imports steam hot tank through seven roller drafting machines and carries out
Then drafting silk is cooled to room temperature by three-level hot gas spring in the case where keeping tension state, winding obtains finished silk.Above-mentioned each section of drawing-off
The tensile property of condition and finished silk is listed in table 1.
Embodiment 2:
Take 51 kilograms of polyvinyl resin with super-high molecular weight powder and 49 kilograms of alkane solvent it is thermally conductive in closed double-jacket
First time physical mixed is carried out in the high-speed mixer of oil heating；Wherein, polyvinyl resin with super-high molecular weight powder is divided equally again
Son amount is 6,000,000, the side chain number of molecular weight distribution 4.0, every 10000 carbon atoms is 1, average grain diameter is 90 micron,
Diameter is distributed as 3.5, average crystallinity 75%；Alkane solvent is nonane, and relative density at room temperature is under 0.72, normal pressure
Boiling point be 150 DEG C；Stirring rate in high-speed mixer is 900rpm, and pressure is 2.8 atmospheric pressure, and temperature is 100 DEG C；It is mixed
Stop stirring after closing 50 minutes, mixture is taken out in release, stand, balance to room temperature, using the sieve of 180 mesh carry out sieving, from
The heart obtains the mixture that nonane content is about 4.9wt%；Take 8 kilograms of this mixture and 92 kilograms of paraffin oil and antioxidant 1,000
Gram, 2.5 kilograms of lubricant second of physical mixed is carried out in closed stirred tank, the stirring rate in stirred tank be 10rpm,
Temperature is 100 DEG C；Mixing 30 minutes after, by slurry injection screw diameter be 95mm, the double screw extruder that draw ratio is 70, material
Cylinder temperature is 180~260 DEG C, screw speed 250rpm；Filament spinning component and the hole count that temperature is 260 DEG C are delivered to through metering pump
The spinneret for being 12 for 240, aperture 0.8mm, draw ratio；Extrusion solution passes through the air gap of 6mm, is 5 DEG C into temperature
Cooling bath, gel fiber through drive roll draw with the rate of 5m/min fall into contain silk cylinder, in the air gap to strand apply
Drawing-off；Gel fiber stands 48 hours at room temperature, then carries out preliminary draft at room temperature, and continuity enter containing hydrocarbon clear
The extraction tank and air dry oven of lotion are extracted and are dried, measure dry silk weight average molecular weight be 4,700,000, extraction,
Drawing-off is carried out to strand in drying process；Dry silk imports steam hot tank through seven roller drafting machines and carries out level Four hot gas spring, then exists
It keeps being cooled to room temperature drafting silk under tension state, winding obtains finished silk.The drawing of above-mentioned each section of draw conditions and finished silk
It stretches performance and is listed in table 1.
Embodiment 3:
Take 75 kilograms of polyvinyl resin with super-high molecular weight powder and 25 kilograms of alkane solvent it is thermally conductive in closed double-jacket
First time physical mixed is carried out in the high-speed mixer of oil heating；Wherein, polyvinyl resin with super-high molecular weight powder is divided equally again
Son amount is 4,500,000, the side chain number of molecular weight distribution 3.0, every 10000 carbon atoms is 0.5, average grain diameter is 50 microns,
Particle diameter distribution is 2.5, average crystallinity 65%；Alkane solvent is dodecane, relative density at room temperature is 0.749,
Boiling point under normal pressure is 216 DEG C；Stirring rate in high-speed mixer is 500rpm, and pressure is 2.0 atmospheric pressure, temperature 60
DEG C: stop stirring after mixing 90 minutes, mixture is taken out in release, stands, balances to room temperature, is sieved using the sieve of 210 mesh
Filter, centrifugation, obtain the mixture that dodecane content is about 2.5wt%；Take 88 kilograms of 12 kilograms of this mixture and mineral oil and
1 kilogram of antioxidant, 1.5 kilograms of antistatic agent second of physical mixed, the stirring in stirred tank are carried out in closed stirred tank
Rate is 35rpm, and temperature is 20 DEG C；Mixing after twenty minutes, by slurry injection screw diameter be 80mm, double spiral shells that draw ratio is 60
Bar extruder, barrel temperature are 180~250 DEG C, screw speed 150rpm；The spinning that temperature is 250 DEG C is delivered to through metering pump
Silk component and the spinneret that hole count is 360, aperture 0.6mm, draw ratio are 10；Extrusion solution passes through the air gap of 10mm,
The cooling bath for being 15 DEG C into temperature, gel fiber, which draws to fall into the rate of 15m/min through drive roll, contains silk cylinder, between air
Drawing-off is applied to strand in gap；Gel fiber stands 32 hours at room temperature, then carries out preliminary draft at room temperature, and continuity
It is extracted and is dried into the extraction tank containing agent for carbon hydrogen detergent and air dry oven, the weight average molecular weight for measuring dry silk is
3790000, drawing-off is carried out to strand in extraction, drying process；Dry silk imports steam hot tank through seven roller drafting machines and carries out three-level
Then drafting silk is cooled to room temperature by hot gas spring in the case where keeping tension state, winding obtains finished silk.Above-mentioned each section of draw conditions
And the tensile property of finished silk is listed in table 1.
Embodiment 4:
Take 87 kilograms of polyvinyl resin with super-high molecular weight powder and 13 kilograms of alkane solvent it is thermally conductive in closed double-jacket
First time physical mixed is carried out in the high-speed mixer of oil heating；Wherein, polyvinyl resin with super-high molecular weight powder is divided equally again
Son amount is 3,000,000, the side chain number of molecular weight distribution 2.0, every 10000 carbon atoms is 0.8, average grain diameter is 30 microns,
Particle diameter distribution is 2.0, average crystallinity 75%；Alkane solvent is decane, and relative density at room temperature is 0.73, normal pressure
Under boiling point be 174 DEG C；Stirring rate in high-speed mixer is 900rpm, and pressure is 2.8 atmospheric pressure, and temperature is 100 DEG C；
Stop stirring after mixing 50 minutes, mixture is taken out in release, stand, balance to room temperature, using the sieve of 210 mesh carry out sieving,
Centrifugation, obtains the mixture that decane content is about 1.3wt%；Take 8 kilograms of this mixture and 92 kilograms of mineral oil and antioxidant 1
Kilogram, 1 kilogram of ultra-violet stabilizer second of physical mixed is carried out in closed stirred tank, the stirring rate in stirred tank is
10rpm, temperature are 100 DEG C；After ten minutes, by slurry injection screw diameter be 95mm, the twin-screw that draw ratio is 60 squeezes for mixing
Machine out, barrel temperature are 180~250 DEG C, screw speed 250rpm；The spinning group that temperature is 250 DEG C is delivered to through metering pump
The spinneret that part and hole count are 480, aperture 0.6mm, draw ratio are 12；Extrusion solution passes through the air gap of 6mm, into temperature
The cooling bath that degree is 15 DEG C, gel fiber, which draws to fall into the rate of 5m/min through drive roll, contains silk cylinder, right in the air gap
Strand applies drawing-off；Gel fiber stands 16 hours at room temperature, then carries out preliminary draft at room temperature, and continuity enter and contain
There are the extraction tank of agent for carbon hydrogen detergent and air dry oven to be extracted and dried, the weight average molecular weight for measuring dry silk is 2,650,000,
Drawing-off is carried out to strand in extraction, drying process；Dry silk imports steam hot tank through seven roller drafting machines and carries out three-level hot gas spring,
Then drafting silk is cooled to room temperature in the case where keeping tension state, winding obtains finished silk.Above-mentioned each section of draw conditions and finished product
The tensile property of silk is listed in table 1.
Embodiment 5:
Take 75 kilograms of polyvinyl resin with super-high molecular weight powder and 25 kilograms of alkane solvent it is thermally conductive in closed double-jacket
First time physical mixed is carried out in the high-speed mixer of oil heating；Wherein, polyvinyl resin with super-high molecular weight powder is divided equally again
Son amount is 4,500,000, the side chain number of molecular weight distribution 4.0, every 10000 carbon atoms is 0.6, average grain diameter is 90 microns,
Particle diameter distribution is 1.5, average crystallinity 65%；Alkane solvent is hendecane, and relative density at room temperature is 0.74, often
The boiling point of pressure is 196 DEG C；Stirring rate in high-speed mixer is 500rpm, and pressure is 2.0 atmospheric pressure, temperature 60
℃；Stop stirring after mixing 90 minutes, mixture is taken out in release, stands, balances to room temperature, is sieved using the sieve of 180 mesh
Filter, centrifugation, obtain the mixture that hendecane content is about 2.5wt%；Take 88 kilograms of 12 kilograms of this mixture and mineral oil and
1 kilogram of antioxidant, 2 kilograms of antistatic agent second of physical mixed is carried out in closed stirred tank, stirring in stirred tank speed
Rate is 35rpm, and temperature is 60 DEG C；Mixing after twenty minutes, by slurry injection screw diameter be 65mm, the twin-screw that draw ratio is 70
Extruder, barrel temperature are 180~260 DEG C, screw speed 350rpm；The spinning that temperature is 250 DEG C is delivered to through metering pump
The spinneret that component and hole count are 360, aperture 1.0mm, draw ratio are 8；Extrusion solution passes through the air gap of 2mm, enters
The cooling bath that temperature is 25 DEG C, gel fiber, which draws to fall into the rate of 15m/min through drive roll, contains silk cylinder, in the air gap
Drawing-off is applied to strand；Gel fiber stands 48 hours at room temperature, then carries out preliminary draft at room temperature, and continuity enter
Extraction tank and air dry oven containing agent for carbon hydrogen detergent are extracted and are dried, and the weight average molecular weight for measuring dry silk is 355
Ten thousand, drawing-off is carried out to strand in extraction, drying process；Dry silk imports steam hot tank progress three-level heat through seven roller drafting machines and leads
It stretches, is then cooled to room temperature drafting silk in the case where keeping tension state, winding obtains finished silk.
The tensile property of above-mentioned each section of draw conditions and finished silk is listed in table 1.
The main draw conditions of table 1 and finished silk tensile property
Claims (10)
1. a kind of superelevation is strong, the preparation method of Gao Mo, fine count fiber, comprising the following steps:
Polyvinyl resin with super-high molecular weight powder and relative density at room temperature are lower than 0.75g/cm by step (1)3And it is boiled under normal pressure
Solvent A of the point higher than 100 DEG C carries out first time physical mixed；
The mixture that step (2) obtains step (1) stands, balances to room temperature, then removes attachment removal through sieving, centrifugation
Extra solvent A in polyvinyl resin with super-high molecular weight powder surface；
The mixture and solvent B and additive that step (3) obtains step (2) carry out second of physical mixed, are mixed into mixing
Slurry；
The mixed slurry that step (4) obtains step (3) injects double screw extruder, passes through metering pump, filament spinning component and spinneret
Plate squeezes out, and enters in circulating cooling water-bath through the air gap, and gel fiber, which is orderly fallen into, under the traction of drive roll contains silk cylinder.
The gel fiber that step (4) obtains is stood 16~48 hours by step (5) at room temperature, is then led in advance at room temperature
Stretch, and continuity enter extraction tank and drying box and extracted and dried；
The drying silk that step (6) obtains step (5) imports steam hot tank through drafting machine and carries out multistage hot gas spring, is then protecting
It holds and is cooled to room temperature drafting silk under tension state, winding obtains finished silk.
2. preparation method according to claim 1, it is characterised in that: in step (1), the ultra-high molecular weight polyethylene
The weight average molecular weight of toner is 3,000,000~6,000,000, and molecular weight distribution is 2.0~4.0, the side chain of every 10000 carbon atoms
Number is 0.1~1；Preferably, average grain diameter is 10~90 microns, particle diameter distribution is 1.5~3.5, and average crystallinity is
55%~75%；Further preferably, the average grain diameter of the polyvinyl resin with super-high molecular weight powder is 10~50 microns, grain
Diameter is distributed as 1.5~2.5.
3. preparation method according to claim 1, it is characterised in that: in step (1), the solvent A is carbon atom number
For one or more mixtures of 7~12 alkane.
4. preparation method according to claim 1,2 or 3, it is characterised in that: in step (1), the super high molecular weight
The weight ratio of polyethylene resin powder and solvent A is 51/49~99/1；Preferably, polyvinyl resin with super-high molecular weight powder
The weight ratio of end and solvent A is 75/25~99/1.
5. preparation method according to claim 1,2,3 or 4, it is characterised in that: in step (1), the first time object
Reason is blended in closed band or 3 has in the container of agitating device and pressure and temperature control and carry out, and stirring rate is 100~
900rpm, pressure are 1.2~2.8 atmospheric pressure, and temperature is 20~100 DEG C, and incorporation time is 10~90 minutes.
6. preparation method according to claim 1, it is characterised in that: in step (2), use mesh number for 180~240 sieve
Net carries out sieving, and finally the weight content in toner is 0.1%~4.9% to the solvent A；Preferably, final
Weight content of the solvent A in polyvinyl resin with super-high molecular weight powder is 0.1%~2.5%.
7. preparation method according to claim 1, it is characterised in that: in step (3), the solvent B is paraffin oil, mine
One of object oil, kerosene or mixture that is any number of and arbitrarily matching；The additive includes antioxidant, lubricant, resists
Electrostatic agent, ultra-violet stabilizer；Wherein, the weight ratio of step (2) obtains mixture and solvent B is 8/92~16/84, is added
Add agent content≤5wt%；
Second of physical mixed is carried out in closed have in agitating device and temperature controlled container, stirring rate
For 10~60rpm, temperature is 20~100 DEG C, and incorporation time is 10~30 minutes.
8. preparation method according to claim 1, it is characterised in that: in step (4), the spiral shell of the double screw extruder
Shank diameter is 65~95mm, and draw ratio is 60~80, and barrel temperature is 180~260 DEG C, and screw speed is 150~350rpm；Institute
The temperature of the filament spinning component and spinneret stated is 240~260 DEG C；The spinneret is round spinneret, hole count is 240~
480, aperture is 0.6~1.0mm, and draw ratio is 8~12；The air gap length is 2~10mm, and cooling bath temperature is
5~25 DEG C, the draw-down rate of drive roll is 5~25m/min；Preferably, the air gap length is 2~6mm, and
Drawing-off is applied to strand in the air gap, draw ratio DR1 is 4~6.
9. preparation method according to claim 1, it is characterised in that: in step (5), the preliminary draft ratio DR2 be 8~
12；Extractant in the extraction tank is one of agent for carbon hydrogen detergent, gasoline, methylene chloride, carbon tetrachloride or any number of
And the mixture arbitrarily matched；Drawing-off is carried out to strand in extraction, drying process, draw ratio DR3 is 1.2~1.6.
10. preparation method according to claim 1, it is characterised in that: in step (6), the drafting machine is that seven rollers are led
Stretch machine；1~3 traction roller of the seven roller drafting machines in neighbouring hot tank side is hot-rolling, the temperature of roll surface temperature and hot tank inlet
It spends consistent；Preferably, the multistage hot gas spring is three-level hot gas spring, draw ratio DR4 is 6~9.
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Cited By (1)
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| CN113529212A (en) * | 2021-06-28 | 2021-10-22 | 上海化工研究院有限公司 | Method and device for quickly separating solvent from ultrahigh molecular weight polyethylene fiber |
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