CN1067731C - Continuous preparation of homogeneous solution of superhigh molecular weight polythene - Google Patents
Continuous preparation of homogeneous solution of superhigh molecular weight polythene Download PDFInfo
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Abstract
The present invention relates to continuous preparation of a homogeneous solution of ultrahigh molecular weight polyethylene, which belongs to the class of high molecules. Alkane solvent is moderately swelled under the corresponding swelling condition of the alkane solvent to prepare suspension liquid of ultrahigh molecular weight polyethylene, and the suspension liquid is continuously and quantitatively fed in a twin-screw extruder under the states of room temperature and atmospheric pressure to complete the process of swelling, dissolution, deaeration and measurement output for continuously preparing a homogeneous spanning solution. The method omits a complicated feeding device and a twin-screw vacuum deaeration device, avoids the occurrence of thermal oxidative degradation and is a rapid, high-efficiency and energy-saving method for continuously preparing the homogeneous spanning solution of the ultrahigh molecular weight polyethylene.
Description
The invention relates to a kind of continuous preparation method of macromolecule homogeneous solution, more particularly about a kind of continuous preparation method of extra-high molecular weight polythene uniform solution.
The continuous preparation of extra-high molecular weight polythene uniform solution is that polyethylene gel spins one of key of spinning with plasticising, and it directly influences the key factors such as mechanical property, production cost, efficient and equipment input of gained fiber.
As everyone knows, polyethylene lacks good solvent, raising along with molecular weight of polyethylene, its solubility property in solvent significantly descends, soluble concentration reduces, and needs long-time heat to finish, and poly thermalization degraded is inevitable in course of dissolution, cause molecular weight distribution to broaden, jeopardize the mechanical property of gained fiber thus; As adopt the dissolving of still formula the time weissenberg phenomenon (being commonly called as rod climbing phenomenon) can take place, cause that the reason of rod climbing phenomenon is that solution viscosity is increased sharply in the course of dissolution.Unique solution route is to reduce solution concentration and lower mixing speed, and the former has obviously improved production cost, and the latter prolongs course of dissolution, causes the inhomogeneities of solution.This shows that the dissolving of still formula is difficult to be accepted by suitability for industrialized production.
For solving the uniform dissolution problem of ultra-high molecular weight polyethylene, people have utilized the good mixing ability of double screw extruder, the uniform dissolution that is used for ultra-high molecular weight polyethylene, though obtained certain effect, but also expose some problems, technology and equipment having been proposed very high requirement, can run into all difficulties in implementation process, especially is the dissolving of the ultra-high molecular weight polyethylene of solvent to alkane.
U.S. Allied company is at US-4, adopts ultra-high molecular weight polyethylene predissolve in Valelinum Liquidum in 413,110, utilizes the double helix blender with its further dissolving again, makes the slurry with viscosity higher and forces in the input double screw extruder and finish dissolving; This technology is the deficiency that remedies the dissolving of twin-screw to the processing intent of predissolve, be that the time of staying of feed liquid in double screw extruder is comparatively of short duration, there is poly thermal oxidative degradation in predissolve to ultra-high molecular weight polyethylene on technology, very complicated on the equipment.Wherein the double helix blender is a high temperature pressure vessel, prepares very difficultly, and there are trouble through the double helix blender in the preparation of slurry and slurry to the coupling of twin-screw input in the operation.
For solving the defective that above-mentioned patent exists, Allied company is again at US-4,784,820 have released new technology route, it is to adopt ultra-high molecular weight polyethylene to form slurry in Valelinum Liquidum, and is even for reaching the concentration of polyethylene in slurry, has used the drum-type blender of (1725 rev/mins) at a high speed, make input feed liquid homogenising, and under the certain pressure condition, import single screw rod with plunger displacement pump and dissolve.The slurry homogenising and the dosing device of this process using can cause numerous difficulties in suitability for industrialized production, the safety and stablization effect of production is particularly outstanding, and the output pressure of screw rod is also on the low side, are unfavorable for stablizing the carrying out of spinning.
Japan Kuraray company proposed two kinds of methods that prepare the ultra-high molecular weight polyethylene uniform spinning solution continuously in 1986.One is JP-86-73743, and detailed process is with ultra-high molecular weight polyethylene first swelling in petroleum solvent, and dissolving just again will be dissolved in double screw extruder without abundant dissolved matter then, make uniform spinning solution thus.Analyze this technical process: ultra-high molecular weight polyethylene stands high temperature for a long time in dissolving tank, cause molecular weight degradation, though nitrogen protection suppresses macromolecules degradation, can not stop the generation of this process.Course of dissolution causes that a large amount of bubbles sneak into, and must carry out deaeration thereafter, and still formula deaeration poor effect, thereby influenced normally carrying out of spinning; Viscosity behind preliminarily solubilised is increased sharply, seriously influence super high molecular polyethylene solution and in twin-screw, import equably continuously, though adopt booster pump can overcome some obstacles, the mutual matching problem of bringing between the two thereupon: export too fast, through being cooled to frozen glue, be difficult for the feeding twin-screw; Export too slowly, can not satisfy the output of twin-screw.The existence of the problems referred to above certainly will influence the continuous and uniformity of its process, more main problem is ultra-high molecular weight polyethylene time of staying in slurry tank and dissolving tank to be difficult to equilibrium, cause that swelling is different with dissolution degree, can finally influence the uniformity of solution undoubtedly, along with the raising of dissolved ultra-high molecular weight polyethylene molecular weight, it is more outstanding that this contradiction can seem.It two is JP-86-143439, specific operation process is with ultra-high molecular weight polyethylene swelling in petroleum solvent, feed quantitatively afterwards that double screw extruder dissolves and be provided with defoaming device in the twin-screw exit, be pressurized to after 20～50 kilograms per centimeter 2 by feed liquid that volume discharges suddenly and vacuum exhaust reaches removal by the bubble of sneaking in the course of dissolution.Analyze this technical process: (1) course of dissolution has a large amount of bubbles and sneaks into, be provided with defoaming device in double screw extruder, though by exhaust apparatus energy exclusive segment bubble, exhaust outlet vacuum height is depended in exhaust, the vacuum height helps deaeration, but solvent also can be overflowed thereupon; The low solvent of vacuum is overflowed and can be controlled, but the deaeration effect obviously reduces.The rising of the main dependence feed pressure of deaeration, the raising of pressure are of value to deaeration to be carried out, yet can cause that also feed liquid overflows at exhaust outlet, influences the uniformity of continuous-dissolution.(2) by the pressure sharp fall of feed liquid after the deaeration, for reaching spinning requirement, must improve feed pressure once more, this wastes the draw ratio of part twin-screw or the output quantity of twin-screw undoubtedly, is affected on usage ratio of equipment.This shows that this technological process can face problems in practical application and expansion production, to seeming more unfavorable in the high polymer solution deaeration of viscosity.
The objective of the invention is to overcome the defective of the continuous preparation ultra-high molecular weight polyethylene spinning solution of prior art, solve that it produces in manufacture craft such as influencing the continuous-dissolution uniformity, problem and thermal oxidative degradation generation problems such as solution deaeration, thus a kind of quick, efficient and energy-conservation continuous method for preparing extra-high molecular weight polythene uniform solution is provided.
This and other purpose of the present invention will and be described by following detailed description and further launch and embody.
In the present invention, the continuous preparation method of extra-high molecular weight polythene uniform solution comprises the employing double screw extruder, may further comprise the steps:
A, ultra-high molecular weight polyethylene carry out swelling in solvent, make the suspension of ultra-high molecular weight polyethylene, and the weight average molecular weight of described ultra-high molecular weight polyethylene is 1 * 10
6～4.5 * 10
6The concentration of ultra-high molecular weight polyethylene in solvent is 4～30%, described solvent is hydrogenated naphthalene, alkane solvent, as tetrahydronaphthalene, decahydronaphthalenes, kerosene, Valelinum Liquidum and paraffin wax, the swelling time of described ultra-high molecular weight polyethylene in solvent is 10 minutes to 1 hour, temperature is 90～120 ℃, and the swelling multiplying power is 1.5～3.0;
B, under atmospheric pressure state, this suspension is fed double screw extruder continuously, quantitatively, the element in the double screw extruder by carry, mixing, knead and measure screwing element and form, it is T that each temperature of double screw extruder is set at the feeding mouth temperature
SwellingBelow-10 ℃, medium temperature is T
DissolvingAbout ± 10 ℃, outlet temperature is T
DissolvingBelow-10 ℃, the screw speed of double screw extruder is 70～250 rev/mins, and 3～20 minutes time of staying in screw extruder of suspension, the head pressure of double screw extruder is 20 kilograms per centimeter
2More than.
Further, the continuous preparation method of extra-high molecular weight polythene uniform solution of the present invention comprises the employing double screw extruder, may further comprise the steps:
A, ultra-high molecular weight polyethylene carry out swelling in solvent, make the suspension of ultra-high molecular weight polyethylene, and the weight average molecular weight of described ultra-high molecular weight polyethylene is 1.5 * 10
6～3.0 * 10
6, the concentration of ultra-high molecular weight polyethylene in solvent is 6～20%, and described solvent is a kerosene, and the swelling time of described ultra-high molecular weight polyethylene in solvent is 10～30 minutes, and temperature is 100～118 ℃, the swelling multiplying power is 1.8～2.3;
B, under atmospheric pressure state, this suspension is fed double screw extruder continuously, quantitatively, the element in the double screw extruder by carry, mixing, knead and measure screwing element and form, it is T that each temperature of double screw extruder is set at the feeding mouth temperature
SwellingBelow-10 ℃, medium temperature is T
DissolvingAbout ± 10 ℃, outlet temperature is T
DissolvingBelow-10 ℃, the screw speed of double screw extruder is 90～200 rev/mins, and 5～10 minutes time of staying in screw extruder of suspension, the head pressure of double screw extruder is 25～40 kilograms per centimeter
2
In the continuous preparation method of extra-high molecular weight polythene uniform solution of the present invention, in double screw extruder, finish swelling, dissolving, deaeration and metering output, the device that suspension continuously, quantitatively feeds double screw extruder can be plunger displacement pump, measuring pump and flow valve etc., and the device that suspension continuously, quantitatively feeds double screw extruder can be the flow valve of any adjusting and matches with charging hopper with overfall.
Method of the present invention has been saved complicated feeding unit and twin-screw vacuum defoamation device, has avoided the generation of thermal oxidative degradation, is a kind of quick, efficient, energy-conservation continuous method for preparing the ultra-high molecular weight polyethylene uniform spinning solution.
Below further describe the present invention.
The course of dissolution of ultra-high molecular weight polyethylene in solvent can be divided into two stages: swelling and dissolving.In the swelling stage, mainly show as solvent and in ultra-high molecular weight polyethylene, permeate and diffusion, it is that dissolving is crucial uniformly.Yet, swelling is a slow process, reason is that the super high molecular weight condensate of high crystallization has hindered the infiltration of solvent, unsuitable swelling can cause forming on ultra-high molecular weight polyethylene particle top layer a high thickness layer, it had both stoped continuous infiltration and the diffusion of solvent in condensate, hindered again that the big molecule of condensate spreads in solvent in the course of dissolution.The remarkable melting effect of double screw extruder improves dissolved efficiency widely, and ultra-high molecular weight polyethylene solubilized concentration is improved significantly, and full-bodied solution has been created condition for foundation, the deaeration of double screw extruder head pressure afterwards again.Based on the condensate swelling process is a slow process, suspension time of staying in double screw extruder is subjected to the limitation of screw slenderness ratio, and swelling is an endothermic process very responsive to temperature, only carry out in narrow temperature range, improper causing of swelling can't make uniform spinning solution.The swelling deficiency causes that the ultra-high molecular weight polyethylene dissolving is inhomogeneous; Swelling is too abundant, and the ultra-high molecular weight polyethylene particle can the group of being gathered into, and has hindered the normal evenly feeding of twin-screw, this shows that suitable swelling becomes the key of preparation homogeneous solution.The swelling rate of ultra-high molecular weight polyethylene and swelling temperature and swelling time are closely related, and relevant with the solvent that adopts again: along with the raising of adopting solvent boiling point, the swelling temperature of ultra-high molecular weight polyethylene has rising slightly; And the raising of ultra-high molecular weight polyethylene molecular weight, make its swelling temperature that tangible rising be arranged, swelling time also increases thereupon, and the best swelling temperature decision of the ultra-high molecular weight polyethylene under specific solvent can be decided by swelling DSC curve, specifically sees CN1050884A for details.
The appropriate swelling of ultra-high molecular weight polyethylene is another key of prepared in twin-screw extruder uniform spinning solution, and the degree of swelling can be characterized by the swelling multiplying power.The swelling multiplying power now is defined as:
★ 1: ultra-high molecular weight polyethylene weight is meant ultra-high molecular weight polyethylene suspension after the swelling gained of weighing after the swelling after getting rid of filter in 0.5 hour.
★ 2: the ultra-high molecular weight polyethylene net weight is meant the ultra-high molecular weight polyethylene after the swelling is carried out three extractions (extractant is an industrial naptha) after the swelling, and 70 ℃ are dried to constant weight weighing gained.
In the external world, show as particle through the ultra-high molecular weight polyethylene after the swelling and swell, and pass on change, and the suspension in solvent increases to translucent.
Ultra-high molecular weight polyethylene high temperature with thermal oxidative degradation easily takes place under oxygen contacts, cause molecular weight sharply to descend and the color and luster flavescence, for avoiding the generation of thermal oxidative degradation, except that in solvent, adding the antioxidant, an effectively measure is that the ultra-high molecular weight polyethylene molecular weight is carried out swelling, thereby the carrying out that has suppressed thermal oxidative degradation carries out swelling afterwards in double screw extruder, and dissolving is to carry out under isolated with air.This measure has guaranteed the stable of ultra-high molecular weight polyethylene molecular weight and has prevented broadening of molecular weight distribution that it is that preparation is high-strength, the basic place of high-modulus polyethylene fiber; Guaranteed simultaneously the stable of ultra-high molecular weight polyethylene swelling multiplying power again, and then it is constant that double screw extruder is able to ultra-high molecular weight polyethylene suspension dissolution process condition, overcome JP-86-73743 and JP-86-143439 and the ultra-high molecular weight polyethylene swelling occurred and dissolve the unbalanced phenomena that may occur.
In view of ultra-high molecular weight polyethylene its swelling temperature narrow range in specific solvent, ultra-high molecular weight polyethylene suspension is reduced to T
Swelling-10 ℃, the swelling of ultra-high molecular weight polyethylene has obtained inhibition, so the temperature of ultra-high molecular weight polyethylene suspension feeding double screw extruder can be at T
Swelling-10 ℃ to selecting arbitrarily between the room temperature.Consider that the variations in temperature of this high temperature suspension in storage process can cause the unstability of dissolution process thereafter, the temperature of more desirable suspension input double screw extruder is a room temperature.It is the input of double screw extruder and the key of output coupling that ultra-high molecular weight polyethylene suspension feeds double screw extruder continuously, quantitatively, it continuously, quantitatively feeding unit can adopt plunger displacement pump, measuring pump, flow valve etc., for stablizing the feeding of double screw extruder, more preferably adopt the flow valve that to regulate arbitrarily to match with the charging hopper of having overfall, the excess part can feed back to by circulating pump and store in the still, is achieved thereby it is quantitatively fed.
The abundant swelling of finishing in double screw extruder through the ultra-high molecular weight polyethylene of appropriate swelling, dissolving, deaeration and metering output are by the multiple screwing element in the double screw extruder, as: carry, mixing, knead and measure screwing element and realize.Because ultra-high molecular weight polyethylene is heated in screw cylinder and stands the good mixed and high speed shear that running up of screwing element cause, at first be that ultra-high molecular weight polyethylene is carried out abundant swelling, then dissolve, viscosity of sludge can sharply rise this moment, and in screw rod, progressively form elevated pressures, this propelling with feed liquid causes that trend that pressure rises gradually makes bubble in the course of dissolution by the gap between screwing element and the double screw extruder barrel, discharge from feeding mouth, thereby reached the effect of exhaust.Because the face head of double screw extruder can reach tens kilograms per centimeter
2More than, the pressure reduction of it and feeding mouth, being far longer than with the head vacuum exhaust (is that vacuum reaches only 1 kilograms per centimeter of 760 millimetres of mercury pressure reduction
2) pressure reduction, this method for exhausting also has the function of automatic adjusting capacity except that exhaust effect is splendid, thereby can reach the continous-stable spinning requirement, none fracture of wire phenomenon that causes because of bubble occurs.
Because the restriction that the draw ratio of double screw extruder is made, the time of staying of ultra-high molecular weight polyethylene suspension in double screw extruder also can be limited to.For making the full and uniform dissolving in screw rod of its suspension.The optimization of double screw extruder spinning technique becomes the key element of the dissolved efficiency that improves double screw extruder, output quantity, deaeration etc.Be specially: the temperature of (1) double screw extruder feeding part is correctly set, and can make feeding normally be carried out being uniform state with ultra-high molecular weight polyethylene suspension.The temperature of feeding mouth is unsuitable too high, and to prevent the obstruction of feeding mouth, its feeding mouth temperature is controlled at T
SwellingBelow-10 ℃; Medium temperature should be controlled at T
Dissolving+ 10 ℃, be beneficial to the required energy of ultra-high molecular weight polyethylene dissolving, big molecular energy promptly is diffused in the solvent goes; Double screw extruder delivery outlet temperature should be at T
DissolvingBelow-10 ℃, so that dissolved super high molecular polyethylene solution can be even; (2) output quantity of the screw speed of double screw extruder decision screw rod and the quality of solubility property.It mainly is the shearing that increases dissolved thing that the present invention adopts the purpose of cocurrent and parallel rotation double screw extruder, reach rapidly-soluble effect, when screw speed reaches 70 rev/mins can be to the dissolving that is well on of ultra-high molecular weight polyethylene suspension, the dissolving of ultra-high molecular weight polyethylene was still normal when screw speed reached 250 rev/mins, it is ineffective to the improvement of dissolving further to improve rotating speed, and can cause excessive shear, cause the fracture of macromolecular chain.So general screw speed should be controlled between 70～250 rev/mins.Consider the stable of the even of dissolving and twin-screw output, can between 90～200 rev/mins, select more desirable; (3) time of staying of ultra-high molecular weight polyethylene suspension in double screw extruder is another requirement of uniform dissolution, the quality of the height of molecular weight, dissolution with solvents performance is the principal element that influences the time of staying, along with the raising of using the ultra-high molecular weight polyethylene molecular weight and the reduction of dissolution with solvents performance, it is necessary suitably increasing the time of staying.Ultra-high molecular weight polyethylene suspension was at least 3 minutes in the time of staying of double screw extruder, surpassed 20 minutes and can cause the polyethylene variable color, made fibre property and descended, and the more desirable time of staying is 5～10 minutes.(4) solution viscosity of ultra-high molecular weight polyethylene is very high, generally reaches more than 3000 centipoises, adopts the bubble eliminating in the discontinuous degassing solution can seem very difficult.The athletic meeting of twin-screw threaded block makes solution constantly produce very thin interface, though it gets rid of the good condition that provides to bubble.In the prior art, add to adopt vacuum exhaust can make its bubble overflow increase, but along with screw rod has the requirement of highoutput, solution can not be oversize in the exhaust outlet time of staying, thereby hindered that bubble drains completely in the solution, thereby influence spinning process stable, carry out lastingly.The formation and the eliminating of analysis bubble, the present invention is the pressure that increases super high molecular weight solution, when twin-screw head pressure reaches 20 kilograms per centimeter
2More than, even the viscosity to 5000 of solution centipoise, bubble can move to the little feeding mouth direction of pressure naturally, and discharges from the feeding mouth of double screw extruder by the gap between screw thread and the swivel nut.The foundation of double screw extruder head pressure and stable the stable of spinning technique thereafter played a key effect, consider that all multi-parts after the double screw extruder as the pressure drop of filter, filament spinning component, suitably improve output pressure to 25 kilograms per centimeter of double screw extruder
2Be necessary, with Pressure control in 25～40 kilograms per centimeter
2Between all can make spinning smooth.
Fig. 1 is a super high molecular weight polyethylene gel spinning process schematic flow sheet.
In Fig. 1, symbology: 1-swelling still, 2-ultra-high molecular weight polyethylene and auxiliary agent feeding mouth, 3-solvent feeding mouth, the 4-baiting valve, 5-ultra-high molecular weight polyethylene suspension stores still, 6-flow valve, 7-double screw extruder charging hopper, 8-overflow material circulating pump, 9-double screw extruder spout, the parallel parallel dual-screw extruding machine of 10-, 11-booster pump, the 12-filter, the 13-measuring pump, 14-spinnerets, 15-ultra-high molecular weight polyethylene strand, the 16-quench tank, 17-draws a machine, and the 18-super high molecular weight polyethylene gel spins
In the present invention, refer in particular to as non-, all parts, amount are unit of weight, and embodiment only for explanation, can not limit the scope of the invention.
Embodiment:
With weight average molecular weight is 280 * 10
440 kilograms of ultra-high molecular weight polyethylenes, 0.8 kilogram of the anti-gas agent of hindered phenol (is 0.02 to polyethylene), 460 kilograms of solution inputs that are mixed with 8% concentration of kerosene (boiling point is 185～300 ℃) have in 500 liters of reactors of stirring, this solution is heated to 115 ℃ plays timing, swelling 10 minutes makes the suspension of ultra-high molecular weight polyethylene.
Ultra-high molecular weight polyethylene suspension after swelling is put into and is stored still, and stirring is cooled to below 98 ℃ standby.The appropriate swelling of ultra-high molecular weight polyethylene this moment, the swelling multiplying power is 2.0, but still is graininess, with the obvious layering of kerosene.Under stirring, with in 70 kilograms of/hour charging hoppers that add double screw extruders, adopt following condition can make the spinning solution of ultra-high molecular weight polyethylene continuously, equably this suspension by flow valve, specific as follows:
1,2 * 58 millimeters of double screw extruder diameter and draw ratio: Φ, L/D=48;
2, the form of double screw extruder: cocurrent and parallel double screw extruder;
3, the screwing element form of double screw extruder: carry, mixing, knead, screwing element such as metering.
4, the rotating speed of double screw extruder: 70～200 rev/mins.
5, the temperature of ultra-high molecular weight polyethylene suspension: room temperature.
6, double screw extruder barrel body temperature: 98 ℃ of feeding sections, 180 ℃ of interludes, 170 ℃ of metering deferent segments.
7, suspension time of staying in double screw extruder: 5 minutes.
8, the head pressure of double screw extruder: 5 minutes.
The suspension of ultra-high molecular weight polyethylene can be made uniform ultra-high molecular weight polyethylene spinning solution with above-mentioned condition, this solution can carry out spinning by double screw extruder head die orifice spinnerets (have 50 holes, the aperture is 0.7 millimeter).Obtain homogeneous transparent, bubble-free ultra-high molecular weight polyethylene strand.
As connecting booster pump at the double screw extruder head, filter, measuring pump, filament spinning component, can carry out continuous spinning process, actual conditions is: measure output with 4 position measuring pumps (280 gram/minute), and carry out spinning, quenching by 100 holes (0.7 millimeter in aperture) spinning plate, reel with 10 meters/minute, obtain thus continuously, ultra-high molecular weight polyethylene gel fiber uniformly.
Above-mentioned gel fiber is carried out continuous extraction, drying and ultra-drawing, and can make intensity is high-strength, the high-modulus polyethylene fiber at 2.5 gram/dawn.
Reference examples 1:
The solution concentration proportioning is identical with embodiment, when the swelling multiplying power of the ultra-high molecular weight polyethylene of swelling gained is 1.3, the suspension of this ultra-high molecular weight polyethylene is dissolved by the embodiment condition, can find from the head die orifice source of double screw extruder: ultra-high molecular weight polyethylene fails fully to be dissolved, being embodied in has inhomogeneous strand to occur in the gained gel fiber, also can occur transparent bulk occasionally and be mixed among the strand.
Reference examples 2:
(dissolution conditions and embodiment were basic identical when the ultra-high molecular weight polyethylene suspension feeding double screw extruder that makes by embodiment dissolved, only screw speed is distinguished to some extent), when screw speed is below 60 rev/mins the time, visible this moment, ultra-high molecular weight polyethylene was failed fully dissolving from the strand that the head die orifice of double screw extruder spues, show as strand thickness inequality, gained frozen glue strand presents the tensile property of extreme difference after the quenching, and when rotating speed surpasses 250 rev/mins, do not control as output quantity, above-mentioned identical phenomenon occurs.
Claims (5)
1, a kind of continuous preparation method of extra-high molecular weight polythene uniform solution comprises the employing double screw extruder, it is characterized in that may further comprise the steps:
A, ultra-high molecular weight polyethylene carry out swelling in solvent, make the suspension of ultra-high molecular weight polyethylene, and the weight average molecular weight of described ultra-high molecular weight polyethylene is 1 * 10
6～4.5 * 10
6The concentration of ultra-high molecular weight polyethylene in solvent is 4～30%, described solvent is hydrogenated naphthalene, alkane solvent, as tetrahydronaphthalene, decahydronaphthalenes, kerosene, Valelinum Liquidum and paraffin wax, the swelling time of described ultra-high molecular weight polyethylene in solution is 10 minutes to 1 hour, temperature is 90～120 ℃, and the swelling multiplying power is 1.5～3.0;
B, under atmospheric pressure state, this suspension is fed double screw extruder continuously, quantitatively, the element in the double screw extruder by carry, mixing, knead and measure screwing element and form, it is T that each temperature of double screw extruder is set at the feeding mouth temperature
SwellingBelow-10 ℃, medium temperature is T
DissolvingAbout ± 10 ℃, outlet temperature is T
DissolvingBelow-10 ℃, the screw speed of double screw extruder is 70～250 rev/mins, and 3～20 minutes time of staying in screw extruder of suspension, the head pressure of double screw extruder is 20 kilograms per centimeter
2More than.
2, the continuous preparation method of extra-high molecular weight polythene uniform solution as claimed in claim 1 comprises the employing double screw extruder, it is characterized in that may further comprise the steps:
A, ultra-high molecular weight polyethylene carry out swelling in solvent, make the suspension of ultra-high molecular weight polyethylene, and the weight average molecular weight of described ultra-high molecular weight polyethylene is 1.5 * 10
6～3.0 * 10
6, the concentration of ultra-high molecular weight polyethylene in solvent is 6～20%, and described solvent is a kerosene, and the swelling time of described ultra-high molecular weight polyethylene in solvent is 10～30 minutes, and temperature is 100～118 ℃, the swelling multiplying power is 1.8～2.3;
B, under atmospheric pressure state, this suspension is fed double screw extruder continuously, quantitatively, the element in the double screw extruder by carry, mixing, knead and measure screwing element and form, it is T that each temperature of double screw extruder is set at the feeding mouth temperature
SwellingBelow-10 ℃, medium temperature is T
DissolvingAbout ± 10 ℃, outlet temperature is T
DissolvingBelow-10 ℃, the screw speed of double screw extruder is 90～200 rev/mins, and 5～10 minutes time of staying in screw extruder of suspension, the head pressure of double screw extruder is 25～40 kilograms per centimeter
2
3, the continuous preparation method of extra-high molecular weight polythene uniform solution as claimed in claim 1 or 2 is characterized in that ultra-high molecular weight polyethylene suspension finishes swelling, dissolving, deaeration and metering output in double screw extruder.
4, the continuous preparation method of extra-high molecular weight polythene uniform solution as claimed in claim 1 or 2 is characterized in that the device that suspension continuously, quantitatively feeds double screw extruder can be plunger displacement pump, measuring pump and flow valve etc.
5, the continuous preparation method of extra-high molecular weight polythene uniform solution as claimed in claim 1 or 2 is characterized in that device that suspension continuously, quantitatively feeds double screw extruder can be the flow valve of any adjusting and matches with charging hopper with overfall.
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| CN97106768A CN1067731C (en) | 1997-12-10 | 1997-12-10 | Continuous preparation of homogeneous solution of superhigh molecular weight polythene |
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| CN97106768A CN1067731C (en) | 1997-12-10 | 1997-12-10 | Continuous preparation of homogeneous solution of superhigh molecular weight polythene |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101967686A (en) * | 2010-09-21 | 2011-02-09 | 中国科学院宁波材料技术与工程研究所 | Method for preparing ultra-high molecular weight polyethylene fiber spinning solution |
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| ES2314299T3 (en) * | 2003-12-19 | 2009-03-16 | SINOTEX INVESTMENT & DEVELOPMENT CO., LTD. | A PROCEDURE TO PREPARE ULTRA-HIGH MOLECULAR WEIGHT POLYETHYLENE FIBERS. |
| CN1256366C (en) * | 2004-11-29 | 2006-05-17 | 北京特斯顿新材料技术发展有限公司 | Method for continuous preparation and mixture of super high molecular polyethylene solution |
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| CN108441971A (en) * | 2018-05-23 | 2018-08-24 | 史小军 | High-strength high-modulus polyethylene fiber spinning solution preparation facilities |
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| US4413110A (en) * | 1981-04-30 | 1983-11-01 | Allied Corporation | High tenacity, high modulus polyethylene and polypropylene fibers and intermediates therefore |
| US4784820A (en) * | 1986-08-11 | 1988-11-15 | Allied-Signal Inc. | Preparation of solution of high molecular weight polymers |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4413110A (en) * | 1981-04-30 | 1983-11-01 | Allied Corporation | High tenacity, high modulus polyethylene and polypropylene fibers and intermediates therefore |
| US4784820A (en) * | 1986-08-11 | 1988-11-15 | Allied-Signal Inc. | Preparation of solution of high molecular weight polymers |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967686A (en) * | 2010-09-21 | 2011-02-09 | 中国科学院宁波材料技术与工程研究所 | Method for preparing ultra-high molecular weight polyethylene fiber spinning solution |
| CN101967686B (en) * | 2010-09-21 | 2012-04-25 | 中国科学院宁波材料技术与工程研究所 | Method for preparing ultra-high molecular weight polyethylene fiber spinning solution |
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| CN1190137A (en) | 1998-08-12 |
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