CN108385179A - A kind of mesophase pitch based precursor continuous filament yarn preparation process - Google Patents
A kind of mesophase pitch based precursor continuous filament yarn preparation process Download PDFInfo
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- CN108385179A CN108385179A CN201810135869.5A CN201810135869A CN108385179A CN 108385179 A CN108385179 A CN 108385179A CN 201810135869 A CN201810135869 A CN 201810135869A CN 108385179 A CN108385179 A CN 108385179A
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- mesophase pitch
- melt
- based precursor
- preparation process
- filament yarn
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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
-
- 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
- D01D1/10—Filtering or de-aerating the spinning solution or melt
- D01D1/103—De-aerating
-
- 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
- D01D1/10—Filtering or de-aerating the spinning solution or melt
- D01D1/106—Filtering
-
- 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
- D01D4/00—Spinnerette packs; Cleaning thereof
-
- 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
- D01D5/096—Humidity control, or oiling, of 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
- D01D5/16—Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
-
- 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
- D01D7/00—Collecting the newly-spun products
-
- 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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Inorganic Fibers (AREA)
Abstract
A kind of mesophase pitch based precursor continuous filament yarn preparation process send mesophase pitch to screw extruder by feeder；Extruder screw heats mesophase pitch, vacuum deaerator when screw rod is run；The melt for melting deaeration by the way that in metering pump melt conveying to filament spinning component, melt is diverted to spinneret by the spreader of filament spinning component, is squeezed out by the spinneret orifice of spinneret and carries out spinning by screw extruder；The fibre bundle of extrusion molding oils, receives silk after draw roll drawing-off.Vacuum deaerator mouth is located at after whole area in the present invention, on the one hand the melt of fusion zone can be prevented to be evacuated breakdown, and sucking gas is caused to dissolve in melt.Mesophase pitch is melted behind screw melting area and is uniformly mixed under twin-screw shear action completely can form the uniform and thin melt of a floor in slot, at this time can be completely disengaged the bubble inside melt by vacuum deaerator.Production efficiency of the present invention is good, and the performance of the mesophase pitch based precursor prepared is good.
Description
Technical field
The present invention relates to a kind of melt-spun, boundling, drawing-off, the windings of mesophase pitch based precursor continuous filament yarn, and in particular to
A kind of mesophase pitch based precursor continuous filament yarn preparation process.
Background technology
Carbon fiber and its composite material have high specific strength, high ratio modulus, high temperature resistant, corrosion-resistant, creep resistant, conduction, biography
A series of excellent properties such as heat and coefficient of thermal expansion are small.It is compound to can not only be used for structural material carrying, is sent out but also as functional material
Wave other effects.Carbon fiber is broadly divided into two big kind of polyacrylonitrile-based carbon fibre and asphalt base carbon fiber according to raw material.It compares
In polyacrylonitrile-based carbon fibre, asphalt base carbon fiber raw material is easy to get, cost is lower, high conversion rate.And it is easier graphitization, mould
Amount is high, has excellent performance, the relationships such as particularly suitable aerospace state to count the people in heat conduction, conduction etc. as functional material
Raw major areas.
Pitch spinning belongs to melt spinning, and there is presently no the spinning process for fitting entirely into pitch, continue to use substantially
The spinning theory and technology of high polymer, or improved and be allowed to be suitable for Melt Spinning of Pitch.
With Polymers Phase ratio, mesophase pitch melt temperature is high, and viscous flow activation energy is big, belongs to thermally sensitive melt.
Melt viscosity varies with temperature fluctuation, and spinning process is difficult to control.It must be with porous spinneret spinning, porous plate in actual production
Since convection heat losses cause have a temperature gradient on its cross section so that actually the spinning temperature of interstitial hole is than edge
Hole is low, is easier close to edge flowing.And melt flows into component from pipeline, and there are resistance damages from extrusion in spinneret orifice
It loses, will also result in the phenomenon of Internal and external cycle spinneret orifice flow velocity unevenness, spinneret orifice is more, and spinning stabilization is more difficult to keep.Protofilament
Very fragile, tensile strength is less than 10MPa, and elongation at break is less than 0.6%, and the general drawing-off of high polymer and transmission device are not yet
Suitable for mesophase pitch melt spinning.It is that overlapping leads to fracture of wire when uncoiling, knots between preventing adjacent filaments when silk winding, needs
Levels tow intersection is wound at an angle, this generally use controls filar guide and moves axially control adjacent filaments along wire drawing tube
Intersecting angle.In the case that intersecting angle is certain, receipts silk speed is faster, and filar guide speed is faster, be easy to cause fracture of wire.To keep
Stablize, receive silk speed using reducing, reduce spinneret hole count, this is prodigious to reduce production efficiency, also increases precursor post-processing
Difficulty.
Mesophase pitch composition is complicated at present, viscous flow activation energy is big, precursor performance is fragile, leads to mesophase pitch production effect
The technical problem that rate is low, precursor performance is low, post-processing difficulty is big.
Invention content
Present invention aims at a kind of mesophase pitch based precursor continuous filament yarn preparation process is provided, melts and spin in high polymer
On the basis of silk, mesophase pitch low production efficiency, the technical problem that precursor performance is low, post-processing difficulty is big are solved.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of mesophase pitch based precursor continuous filament yarn preparation process, includes the following steps：
Step 1：Mesophase pitch after crushing is sent by feeder to screw extruder；
Step 2：Extruder screw heats mesophase pitch, and bleeding point is arranged after the areas Bing Zhong, and screw rod subtracts when running
Pressure-off is steeped；
Step 3：The melt for melting deaeration is sent into metering pump by screw extruder, then passes through metering pump melt conveying to spinning
In silk component, melt is diverted to spinneret by the spreader of filament spinning component, is squeezed out by the spinneret orifice of spinneret and carries out spinning；
Step 4：The fibre bundle of extrusion molding is oiled by oiling device；
Step 5：Tow receives silk on wire drawing tube, obtaining mesophase pitch based precursor after draw roll drawing-off.
The present invention, which further improves, to be, in step 1, mesophase pitch softening point is 270 DEG C, and interphase content is
100wt%.
The present invention, which further improves, to be, the temperature of the sintering of extruder screw starts to aoxidize less than mesophase pitch
10~30 DEG C of temperature, the temperature in final temperature area is less than 10~30 DEG C of spinning temperature.
The present invention, which further improves, to be, in step 2, the pressure of deaeration is -0.05~-0.1MPa.
The present invention, which further improves, to be, in step 3, filament spinning component includes shell and point being arranged in shell
Flow cone forms runner, strainer and spinneret is disposed at runner exit between spreader and shell；It is provided on strainer
Metal sand.
The present invention, which further improves, to be, having heaters is arranged in hull outside.
The present invention, which further improves, to be, in step 4, oiling device includes two oiling rollers disposed in parallel, each oil
Roller diameter is 150mm, and fibre bundle is in contact with two oiling rollers, and fibre bundle and vertical direction angle are 10~20 °.
The present invention, which further improves, to be, in step 4, two oiling rollers of oiling device are located at side before and after fibre bundle, and
And one high and one low setting.
The present invention, which further improves, to be, tow keeps tow parallel after draw roll drawing-off through draw-off godet, then
It is wound on wire drawing tube, while wire drawing tube is in axially reciprocating.
Compared with prior art, the device have the advantages that：Vacuum deaerator mouth is located at after whole area in the present invention, can
To prevent the melt of fusion zone to be evacuated breakdown, sucking gas is caused to dissolve in melt.Mesophase pitch passes through screw melting area
One layer of uniform and thin melt can be formed in slot by melting and being uniformly mixed under twin-screw shear action completely afterwards, be led at this time
The bubble inside melt can be completely disengaged by crossing vacuum deaerator.To between spinneret orifice after melt and metering pump before metering pump
Melt applies certain pressure by screw extruder and metering pump respectively, it is ensured that melt is closely knit and compresses dissolving inside melt
Bubble, it is possible to reduce fracture of wire.It can be escaped out from filament surfaces in the bubble of melt extrusion spinneret orifice, these high pressures, it can be with
Reduce the hole defect inside precursor.Production efficiency of the present invention is high, and the performance of the mesophase pitch based precursor prepared is good.
Further, extruder screw sintering temperature start oxidizing reaction temperature less than mesophase pitch can be further
The possibility of raw material oxidation deterioration is reduced, whole area's temperature can reduce interphase melt less than spinning temperature and decompose at high temperature instead
It answers.
Further, for filament spinning component by outsourcing heater heating and thermal insulation, this causes spinneret to have inside and outside its cross section
One temperature gradient exists, and the temperature of inner ring hole is lower than outer ring, and cycle hole melt flows are easier, and causes Internal and external cycle tow state not
One spinning is unstable.Since spreader is arranged, Internal and external cycle melt state difference can be reduced using the method for shunting, by group
Inside part plus a spreader, pitch residence time under spinning temperature can be reduced, reducing melt, fluxion strap comes from inside to outside
Pressure gap.
Further, the method to oil is contacted using front and back two sides oiling roller, tow is in vertical direction under oiling roller effect
Certain angle ensures that every silk uniformly oils, and oiling roller can wipe the extra finish of filament surfaces off, and one is formed in fiber surface
The uniform and thin protective film of layer.Oiling roller and tow contact surface are small, and friction is few, reduce abrasion, can be by the monofilament to oil in front and back
Collect upwards bundled together.
Further, two oiling rollers of oiling device are located at side before and after fibre bundle, and one high and one low setting, have both played limit
Position, and tow and oiling roller contact area can be reduced, to reduce friction, ensure that tow fully oils without excessive.
Further, draw-off godet keeps tow to be parallel to wire drawing tube radially winding, wire drawing tube radial rotating winding, while
Axially retain certain speed reciprocating motion so that tow deviates wire drawing tube section certain angle, and different number of plies angle silks intersect volume
Around.The cross winding that tow is realized by the way of fixed draw-off godet, wire drawing tube axially reciprocating, avoid fragile tow because
Transverse movement and fracture of wire reduce precursor abrasion, ensure that the tow uncoiling of winding is smooth, are convenient for post-processing operation.
Description of the drawings
Fig. 1 is the structural schematic diagram of filament spinning component in the present invention.
Wherein, 1 is runner, and 2 be metal sand, and 3 be strainer, and 4 be spinneret, and 5 be spreader.
Specific implementation mode
It is described in detail below by specific embodiment.
For filament spinning component by outsourcing heater heating and thermal insulation, this causes spinneret to have one inside and outside its cross section in the present invention
Temperature gradient exists, and the temperature of inner ring hole is lower than outer ring, and cycle hole melt flows are easier, and Internal and external cycle tow state is caused to differ
Spinning is unstable.Internal and external cycle melt state difference is reduced using the method for shunting, component internal adds a spreader, reduces pitch and exists
The spinning temperature lower residence time reduces the melt pressure gap that fluxion strap comes from inside to outside.
Step 1：Mesophase pitch is ground, feeder feeding to screw extruder is passed through.Wherein, the centre
Asphalt phase softening point is 270 DEG C, and interphase mass content is 100wt%, belongs to methyl naphthalene synthetic asphalts.
Step 2：Extruder screw heats mesophase pitch, and the temperature of sintering starts to aoxidize less than mesophase pitch
10~30 DEG C of temperature, the temperature in final temperature area is more than mesophase pitch softening point temperature and is less than 10~30 DEG C of spinning temperature, and
Bleeding point, vacuum deaerator when screw rod is run are set after whole area, and deaeration pressure is -0.05~-0.1MPa.
Step 3：The melt that extruder will melt deaeration is sent into metering pump, before metering pump pressure between 1~2MPa, and
It is 1.5~5MPa to give spinning pressure by metering pump, by metering pump accurate measurement melt conveying to filament spinning component, spinning
The concrete structure of component is shown in Fig. 1.Filament spinning component includes shell and the spreader being arranged in shell 5, spreader 5 and shell it
Between formed runner 1, the exit of runner 1 is disposed with strainer 3 and spinneret 4.Metal sand 2 is provided on strainer 3,
In, spinneret is 500 holes.
Melt is branched to filament spinning component outer ring by melt by the spreader 5 in filament spinning component, inside filament spinning component
Add a spreader 5 so that melt is squeezed out without among spinneret by outer ring spinneret orifice.Pitch passes through filament spinning component
Interior 2 rectification of metal sand, mixed merga pass strainer 3 filter out the impurity such as bubble, gel, reach spinning temperature.Melt passes through spray
4 outer ring spinneret orifice of filament plate squeezes out.
Step 4：The fibre bundle of extrusion molding is oiled by oiling device, and oiling device includes two oil disposed in parallel
Roller, each a diameter of 150mm of oiling roller, fibre bundle are in contact with two oiling rollers, and fibre bundle and vertical direction angle are 10~20 °,
It can ensure fully to oil, reduce tow and oiling roller contact area, to reduce friction.Two oiling rollers are located at before and after fibre bundle
Side, and one high and one low setting, difference in height 150mm not only play limit but also can ensure that tow fully oils without excessive.
Step 5：Tow draws after draw-off godet draws silk to draw roll drawing-off, then by the draw-off godet on tension sensor
Upper wire drawing tube winding.Thread tension is controlled by pressure sensor, keeps draw roll consistent with wire drawing tube speed.
Draw-off godet keeps tow to be parallel to, and wire drawing tube is radially winding, and wire drawing tube radial rotating is wound, while being axially retained
Certain speed moves back and forth so that tow deviates wire drawing tube section certain angle, different number of plies angle silk cross windings.
Obtained mesophase pitch precursor specification is between 475~500, and for diameter between 14~16um, length is big
In 45Km.
It is 150 DEG C that mesophase pitch in the present invention, which starts oxidizing temperature, and spinning temperature is 330 DEG C.
Embodiment 1
Step 1：Mesophase pitch is ground, is sent to screw extruder by feeder.
Step 2：Mesophase pitch passes through multiple heating region mixed meltings of screw extruder, extruder screw heating
Temperature is 130~310 DEG C.The temperature of sintering is less than 20 DEG C of the temperature that mesophase pitch starts oxidation, and the temperature in final temperature area is
310 DEG C, it is more than mesophase pitch softening point temperature and is less than 20 DEG C of spinning temperature.Bleeding point is set after whole area, opens spiral shell
Vacuum deaerator behind bar extruder final temperature area, and the pressure of vacuum deaerator is -0.1MPa.
Step 3：Screw extruder will melt deaeration melt be sent into metering pump, pump before pressure be maintained at 1.5~2MPa it
Between.By in metering pump accurate measurement melt conveying to filament spinning component, and pressurize.The melt of melting deaeration is shunted by spreader
Outer ring in filament spinning component, spreader are solid so that melt is sprayed without among spinneret by the outer ring of spinneret
Wire hole squeezes out.After squeezing out thread stabilization, spinning pressure is stablized between 3~4MPa.Pitch passes through the gold in filament spinning component
The rectification of category sand, mixed merga pass strainer filtering fall the impurity such as bubble, gel, reach spinning temperature.Wherein, spinneret hole count is
500。
Step 4：The fibre bundle of extrusion molding is oiled by oiling device, and oiling device includes two oil disposed in parallel
Roller, each a diameter of 150mm of oiling roller, fibre bundle are in contact with two oiling rollers, and fibre bundle and vertical direction angle are 10 °.Two
Oiling roller is located at side before and after fibre bundle, and one high and one low setting, not only plays limit but also can ensure that tow fully oils without excessive.
Step 5：Tow draws after draw-off godet draws silk to draw roll drawing-off, then by the draw-off godet on tension sensor
Upper wire drawing tube winding.Thread tension is controlled in 10~20cN by pressure sensor, keeps draw roll consistent with wire drawing tube speed.
Draw-off godet is fixed and radially winding, the wire drawing tube radial rotating winding that keeps tow to be parallel to wire drawing tube, while axially retaining one
Constant speed degree moves back and forth, speed 15.2m/min, and upper and lower tow intersecting angle is 21.6 °, and winding obtains mesophase pitch precursor
Continuous filament yarn.
Obtained mesophase pitch precursor continuous filament yarn average diameter is 15.5um, and radical adds up between 495~500
Continuous length about 96km.
The mesophase pitch graphite fibre tensile strength obtained after 2800 DEG C of graphitization processings is 2735MPa, is stretched
Modulus is 698GPa, and thermal conductivity is 631W/ (mK), and continuous length is more than 2000m.
Embodiment 2
Step 1：Mesophase pitch is ground, is sent to screw extruder by feeder.
Step 2：Mesophase pitch by multiple heating region mixed meltings of screw extruder, heating temperature is 130~
310℃.The temperature of sintering is less than 20 DEG C of the temperature that mesophase pitch starts oxidation, and the temperature in final temperature area is 310 DEG C, in being more than
Between asphalt phase softening point temperature and be less than 20 DEG C of spinning temperature.Bleeding point is set after whole area, opens screw extruder final temperature
Vacuum deaerator behind area, and the pressure of vacuum deaerator is -0.1MPa.
Step 3：Screw extruder will melt deaeration melt be sent into metering pump, pump before pressure be maintained at 1~1.3MPa it
Between.By in metering pump accurate measurement melt conveying to filament spinning component, and pressurize.The melt of melting deaeration is shunted by spreader
Outer ring in filament spinning component, spreader are solid so that melt is sprayed without among spinneret by the outer ring of spinneret
Wire hole squeezes out.After squeezing out thread stabilization, spinning pressure is stablized between 1.5~2.5MPa.Pitch passes through in filament spinning component
Metal sand rectification, mixed merga pass strainer filtering fall the impurity such as bubble, gel, reach spinning temperature.Wherein, spinneret hole count
It is 300.
Step 4：The fibre bundle of extrusion molding is oiled by oiling device, and oiling device includes two oil disposed in parallel
Roller, each a diameter of 150mm of oiling roller, fibre bundle are in contact with two oiling rollers, and fibre bundle and vertical direction angle are 10 °.Two
Oiling roller is located at side before and after fibre bundle, and one high and one low setting, not only plays limit but also can ensure that tow fully oils without excessive.
Step 5：Tow draws after draw-off godet draws silk to draw roll drawing-off, then by the draw-off godet on tension sensor
Upper wire drawing tube winding.Thread tension is controlled in 10~20cN by pressure sensor, keeps draw roll consistent with wire drawing tube speed.
Draw-off godet is fixed and radially winding, the wire drawing tube radial rotating winding that keeps tow to be parallel to wire drawing tube, while axially retaining one
Constant speed degree moves back and forth, speed 15m/min, and intersecting angle is 21.6 °, and winding obtains mesophase pitch precursor continuous filament yarn.
Obtained mesophase pitch precursor continuous filament yarn average diameter is 15um, and radical adds up to connect between 295~300
Continuous length about 120Km.
The mesophase pitch graphite fibre tensile strength obtained after 2800 DEG C of graphitization processings is 2758MPa, is stretched
Modulus is 716GPa, and thermal conductivity is 648W/ (mK), and continuous length is more than 3000m.
Comparative example 1
Step 1：Mesophase pitch is ground, is sent to screw extruder by feeder.
Step 2：Mesophase pitch by multiple heating region mixed meltings of screw extruder, heating temperature is 200~
330 DEG C, 330 areas DEG CWei Zhong temperature.Bleeding point is set after whole area, opens the vacuum deaerator behind screw extruder final temperature area,
And the pressure of vacuum deaerator is -0.1MPa.
Step 3：Screw extruder will melt deaeration melt be sent into metering pump, pump before pressure be maintained at 1.5~2MPa it
Between.By in metering pump accurate measurement melt conveying to filament spinning component, and pressurize.The melt of melting deaeration is shunted by spreader
Outer ring in filament spinning component, spreader are solid so that melt is sprayed without among spinneret by the outer ring of spinneret
Wire hole squeezes out.After squeezing out thread stabilization, spinning pressure is stablized between 3~5MPa.Pitch passes through the gold in filament spinning component
The rectification of category sand, mixed merga pass strainer filtering fall the impurity such as bubble, gel, reach spinning temperature.Wherein, spinneret hole count is
500。
Step 4：The fibre bundle of extrusion molding is oiled by oiling device, and oiling device includes two oil disposed in parallel
Roller, each a diameter of 150mm of oiling roller, fibre bundle are in contact with two oiling rollers, and fibre bundle and vertical direction angle are 10 °.Two
Oiling roller is located at side before and after fibre bundle, and one high and one low setting, not only plays limit but also can ensure that tow fully oils without excessive.
Step 5：Tow draws after draw-off godet draws silk to draw roll drawing-off, then by the draw-off godet on tension sensor
Upper wire drawing tube winding.Thread tension is controlled in 5~10cN by pressure sensor, keeps draw roll consistent with wire drawing tube speed.
Draw-off godet is fixed and radially winding, the wire drawing tube radial rotating winding that keeps tow to be parallel to wire drawing tube, while axially retaining one
Constant speed degree moves back and forth, speed 14.3m/min, and intersecting angle is 21.6 °, and winding obtains mesophase pitch precursor and continuously grows
Silk.
Obtained mesophase pitch precursor continuous filament yarn average diameter is 16um, and radical adds up to connect between 475~500
Continuous length about 45Km.
The mesophase pitch graphite fibre tensile strength obtained after 2800 DEG C of graphitization processings is 1927MPa, is stretched
Modulus is 550GPa, and thermal conductivity is 531W/ (mK), and continuous length is more than 500m.
From embodiment 1,2 and comparative example 1 as can be seen that the mesophase pitch that can obtain better performances using the present invention is former
Silk.
Embodiment 3
Step 1：Mesophase pitch after crushing is sent by feeder to screw extruder；
Step 2：Extruder screw heats mesophase pitch, and bleeding point is arranged after the areas Bing Zhong, and screw rod subtracts when running
Pressure-off is steeped；Wherein, extruder screw heating temperature is 140~300 DEG C, and the temperature of sintering starts to aoxidize less than mesophase pitch
10 DEG C of temperature, the temperature in final temperature area is 300 DEG C, is more than mesophase pitch softening point temperature and is less than 30 DEG C of spinning temperature.It is de-
The pressure of bubble is -0.05MPa.
Step 3：Screw extruder will melt deaeration melt be sent into metering pump, pump before pressure be maintained at 1.5~2MPa it
Between.By in metering pump accurate measurement melt conveying to filament spinning component, and pressurize.The melt of melting deaeration is shunted by spreader
Outer ring in filament spinning component, spreader are solid so that melt is sprayed without among spinneret by the outer ring of spinneret
Wire hole squeezes out.After squeezing out thread stabilization, spinning pressure is stablized between 3~4MPa.Pitch passes through the gold in filament spinning component
The rectification of category sand, mixed merga pass strainer filtering fall the impurity such as bubble, gel, reach spinning temperature.Wherein, spinneret hole count is
500。
Step 4：The fibre bundle of extrusion molding is oiled by oiling device；Oiling device includes two oil disposed in parallel
Roller, each a diameter of 150mm of oiling roller, fibre bundle are in contact with two oiling rollers, and fibre bundle and vertical direction angle are 10 °.Two
Oiling roller is located at side before and after fibre bundle, and one high and one low setting, not only plays limit but also can ensure that tow fully oils without excessive.
Step 5：Tow keeps tow parallel after draw roll drawing-off through draw-off godet, is then wound on wire drawing tube, together
When wire drawing tube in axially reciprocating, obtain mesophase pitch based precursor.
Embodiment 4
Step 1：Mesophase pitch after crushing is sent by feeder to screw extruder.
Step 2：Extruder screw heats mesophase pitch, and bleeding point is arranged after the areas Bing Zhong, and screw rod subtracts when running
Pressure-off is steeped；Wherein, extruder screw heating temperature is 120~320 DEG C, and the temperature of sintering starts to aoxidize less than mesophase pitch
30 DEG C of temperature, the temperature in final temperature area is 320 DEG C, is more than mesophase pitch softening point temperature and is less than 10 DEG C of spinning temperature.It is de-
The pressure of bubble is -0.05MPa.
Step 3：Screw extruder will melt deaeration melt be sent into metering pump, pump before pressure be maintained at 1.5~2MPa it
Between.By in metering pump accurate measurement melt conveying to filament spinning component, and pressurize.The melt of melting deaeration is shunted by spreader
Outer ring in filament spinning component, spreader are solid so that melt is sprayed without among spinneret by the outer ring of spinneret
Wire hole squeezes out.After squeezing out thread stabilization, spinning pressure is stablized between 3~4MPa.Pitch passes through the gold in filament spinning component
The rectification of category sand, mixed merga pass strainer filtering fall the impurity such as bubble, gel, reach spinning temperature.Wherein, spinneret hole count is
500。
Step 4：The fibre bundle of extrusion molding is oiled by oiling device；Oiling device includes two oil disposed in parallel
Roller, each a diameter of 150mm of oiling roller, fibre bundle are in contact with two oiling rollers, and fibre bundle is 20 ° with vertical square angle.Two oil
Roller is located at side before and after fibre bundle, and one high and one low setting, not only plays limit but also can ensure that tow fully oils without excessive.
Step 5：Tow keeps tow parallel after draw roll drawing-off through draw-off godet, is then wound on wire drawing tube, together
When wire drawing tube in axially reciprocating, obtain mesophase pitch based precursor.
Claims (9)
1. a kind of mesophase pitch based precursor continuous filament yarn preparation process, which is characterized in that include the following steps：
Step 1：Mesophase pitch after crushing is sent by feeder to screw extruder；
Step 2：Extruder screw heats mesophase pitch, bleeding point is arranged after the areas Bing Zhong, decompression is de- when screw rod is run
Bubble；
Step 3：The melt for melting deaeration is sent into metering pump by screw extruder, then passes through metering pump melt conveying to spinning group
In part, melt is diverted to spinneret by the spreader of filament spinning component, is squeezed out by the spinneret orifice of spinneret and carries out spinning；
Step 4：The fibre bundle of extrusion molding is oiled by oiling device；
Step 5：Tow receives silk on wire drawing tube, obtaining mesophase pitch based precursor after draw roll drawing-off.
2. a kind of mesophase pitch based precursor continuous filament yarn preparation process according to claim 1, which is characterized in that step
In one, mesophase pitch softening point is 270 DEG C, and interphase content is 100wt%.
3. a kind of mesophase pitch based precursor continuous filament yarn preparation process according to claim 1, which is characterized in that squeeze out
The temperature of the sintering of machine screw rod is less than 10~30 DEG C of the temperature that mesophase pitch starts oxidation, and the temperature in final temperature area is less than spinning
10~30 DEG C of temperature.
4. a kind of mesophase pitch based precursor continuous filament yarn preparation process according to claim 1, which is characterized in that step
In two, the pressure of deaeration is -0.05~-0.1MPa.
5. a kind of mesophase pitch based precursor continuous filament yarn preparation process according to claim 1, which is characterized in that step
In three, filament spinning component includes shell and the spreader being arranged in shell (5), and spreader (5) forms runner between shell
(1), runner (1) exit is disposed with strainer (3) and spinneret (4)；Metal sand (2) is provided on strainer (3).
6. a kind of mesophase pitch based precursor continuous filament yarn preparation process according to claim 5, which is characterized in that shell
Having heaters is arranged in outside.
7. a kind of mesophase pitch based precursor continuous filament yarn preparation process according to claim 1, which is characterized in that step
In four, oiling device includes two oiling rollers disposed in parallel, each a diameter of 150mm of oiling roller, and fibre bundle connects with two oiling rollers
It touches, fibre bundle and vertical direction angle are 10~20 °.
8. a kind of mesophase pitch based precursor continuous filament yarn preparation process according to claim 7, which is characterized in that step
In four, two oiling rollers of oiling device are located at side before and after fibre bundle, and one high and one low setting.
9. a kind of mesophase pitch based precursor continuous filament yarn preparation process according to claim 1, which is characterized in that tow
It keeps tow parallel through draw-off godet after draw roll drawing-off, is then wound on wire drawing tube, while wire drawing tube is in axial reciprocating
Movement.
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