CN1060543C - Method and apparatus for continuous making superhigh molecula polyethylene fibre - Google Patents
Method and apparatus for continuous making superhigh molecula polyethylene fibre Download PDFInfo
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Abstract
The present invention relates to a continuous preparation method for ultra high molecular weight polyethylene fibers and equipment specially designed for implementing the method. In the method, a powdery ultra high molecular weight polymer is pre-swelled in a pre-swelling kettle provided with a novel stirrer and a baffle plate to prepare a suspended solution, and then, the suspended solution is continuously and stably conveyed into a twin-screw extruder by a metering pump and rapidly converted into a homogeneous jel solution subsequently extruded, spun and molded. Due to the novel stir structure in the method, the method has the advantages of high mix efficacy, no dead angle of a material system, no deposition and obvious resistance reduction and is especially suitable for preparing fibers with ultra high intensity and ultra high modulus in the mode of the powdery high molecular weight polymer as raw materials.
Description
What the present invention relates to is continuous preparation method of a kind of superhigh molecular weight polyethylene fibers and the equipment that is used for this method.
In recent years, about making frozen glue solution, spinning, desolventizing with powdery UHMW-PE condensate, surpassing the method that high strength, high modulus fibre are produced in times hot-stretch, many patent reports have been arranged, as USP4413110, USP4422993, USP4430223, USP4436689 etc.
Chinese patent CN85107352A also discloses the end content of a part of this respect.
Above-mentioned patent disclosure elder generation with the polymer solvent swell, import mixing in the extruder (or blender) then, import the method for double screw extruder extruding spinning again;
In addition, Japan Patent also discloses the content of this respect, as JP62-257414 etc.; This patent proposes solvent and mixing of materials are evenly directly injected the double screw extruder dissolving spinning in the back;
The fiber that adopts above-mentioned disclosed method to obtain, owing to have excellent properties such as high-strength, Gao Mo, the demand of industry be can satisfy, the required rope of each industrial circle, cable, rope, net, band, protection, defence apparatus and clothes, MISSILE LAUNCHING, sports goods and facility, Offshore Units etc. are applied to fiber.
Although above-mentioned patent all discloses some concrete grammars, but still have weak point.As: these methods have complex process, the cycle is long, equipment investment is high, the ribbon evenness is difficult for troublesome poeration stable and that bring thus.
At the defective that above-mentioned patent exists, propose in the Chinese patent 93244821.6 to use the compound screw ribbon agitator to carry out the preparation of frozen glue solution.We are at industrial practical research initial stage the mid-80, and find with this class agitator (two helical ribbon agitator) preparation frozen glue solution: this method is not suitable for continuously, preparation of industrialization in batches.Mainly show:
1, in dissolution kettle, super high molecular weight polymer is carried out formulations prepared from solutions, come down to have experienced pre-swelling, frozen glue tackify, homogenizing insulation, deaeration, metering and extrude course of conveying.Each process all needs temperature control speed and mixing speed strict coupling control, especially frozen glue tackify stage in each stage simultaneously to the requirement difference of mixing speed, power of agitator, heating rate, temperature control etc.
2, solution system frozen glue tackify process is to carry out under stirring, because polymer molecular weight height, viscosity are big, even adopt the compound screw ribbon agitator to still have rod-climbing effect to exist, the existence of this effect is the principal element that influences homogeneous frozen glue formulations prepared from solutions.
3, owing to take off to the greatest extent in the very difficult frozen glue solution behind tackify of the bubble that stirring produces, remove bubble length consuming time, residual not most bubble is brought spinning solution into will cause cavity filament and fracture of wire.
4, heavy polymer frozen glue solution is the elastico-viscous body with higher elasticity and viscosity.The frozen glue solution that is made by dissolution kettle is difficult to directly enter double screw extruder, easy general material.
5, technology intermittently, material can not thoroughly drain frequent, time-consuming, the effort of kettle cleaning in the still.
6, the frozen glue stability of solution that makes poor (between criticizing and criticizing), strand are unfavorable for stable batch process the in batches.
The purpose of this invention is to provide a kind of superhigh molecular weight polyethylene fibers method of preparation continuously, specifically, the object of the present invention is to provide a kind of can satisfy the industrializing implementation requirement, with powdery super high molecular weight or heavy polymer be raw material with the decahydronaphthalene be solvent continuously in very short time preparation have the frozen glue solution of finite concentration (5%～20%) and the new method that frozen glue formulations prepared from solutions and gel spinning are carried out continuously.
Another object of the present invention be to provide a kind of be applicable to said method, the swelling still that CBY three rachises are flowed compound stirring structure is housed.
Purpose of the present invention can be achieved by following process, method of the present invention be with the powdery polymer of granularity＜200 μ in the swelling still that CBY three rachises flow compound stirring structure is housed, mix pre-swelling with certain amount of solvent, formation has certain density even high polymer suspension; This suspension is transported in the screw extruder by measuring pump, and the quick homogeneous frozen glue solution that forms is measured, extrudes, is shaped in extruder; The gel spun fiber that obtains makes high-strength, high-modulus polyethylene fiber through desolventizing, drying, a super times hot-stretch.
Applicant's result of study shows, adopts the super high molecular weight polymer of powdery to make the key that homogeneous decahydronaphthalene frozen glue solution is realization UHMWPE fiber industryization continuously.
Because the polymer molecular weight height, to the industrializing implementation of the even matter frozen glue solution of serialization preparation all proposed aspect technology, the equipment many overcritical;
In addition, the acquisition of homogeneous frozen glue solution is in the whole process of high-strength, high-modulus polyethylene fiber, and very big to spinnability and the influence of stretching operability, it directly influences the quality stability and the output of semi-finished product and end properties.
Therefore, the continuous preparation of homogeneous decahydronaphthalene frozen glue solution is considerable in suitability for industrialized production.
Be description of drawings below,, can better understanding be arranged the present invention by description to accompanying drawing.
Fig. 1 is the pre-swelling still signal that the CBY of being equipped with three rachises of the present invention are flowed compound agitator and baffle plate
Figure;
Fig. 2 is the subjective figure of CBY axial blade of the present invention;
Fig. 3 is the vertical view of CBY axial blade of the present invention;
Fig. 4 is A-A profile of Fig. 3;
Fig. 5 is a pre-swelling still Internal baffle cutaway view of the present invention;
Fig. 6 is the vertical view of Fig. 5;
Fig. 7 is the swelling curve of powdery ultra-high molecular weight polyethylene under different temperatures that is used to prepare ultra-high molecular weight polyethylene of the present invention, wherein, and " " 70 ℃ among the figure, " " 80 ℃, " ◇ " 90 ℃, " " 93 ℃.
Among the figure: 1. kettle, 2. oil lagging, 3. heat-insulation layer, 4. porous spray thrower, 5. baffle plate,
6. temperature tube, 7. shunting guider, 8. bleeder valve, 9. axle head baffle plate,
10. blade (CBY axial flow), 11.CBY three rachises are flowed compound agitator, 12. kettle covers.
β among Fig. 2aThe root of blade laying angle, βtBe the vane end faces laying angle. Among Fig. 4 from the impeller center to the laying angle β in arbitrary cross section, end of blade different radii placeiPress the uniform pitch structural design.
Shown in Fig. 2,3,4, the blade that uses in this method from end face 13 to root 14 along leaf the wide cambered surface that is, the center line of arbitrary cross section 15 is camber line, the radius of curvature R of this section determines that with the ratio of arc length a its ratio is chosen by the action h of center camber line on this cross section in 0.04-0.08 scope.
Whole blade inlet edge 16 is repaiied the garden, and radius r is half of vane thickness, and trailing edge 17 is also accomplished transition arc, to reduce the resistance of blade.
Next further specify by reference to the accompanying drawings implementation process of the present invention.
Superhigh molecular weight polyethylene fibers continuous production method of the present invention be the industrialization continuous production with powdery UHMWP (ultra-high molecular weight polyethylene) decahydronaphthalene homogeneous frozen glue solution focus on the preswollen equipment and process control of mixing of powdery heavy polymer and continuously, stably on metering conveyor and the technology controlling and process, they are that the basic technology of homogeneous decahydronaphthalene frozen glue solution preparation is crucial.
The pre-swelling of mixing among the preparation method of the present invention refers to whole decahydronaphthalene solvents that heavy polymer and parts by weights are mixed with finite concentration frozen glue solution are dropped into together carries out swelling and all mixed in the pre-swelling still (Fig. 2), make the unit for uniform suspension of super high molecular weight polymer.
The present invention is different with the disclosed method of CN85107352A, and the homogenization of the pre-swelling still of mentioning in the method for the present invention is jointly to finish by the agitator and the baffle plate 5 that are contained in this still.
This agitator 11 is for adapting to method specialized designs processing of the present invention, and concrete is that CBY type three rachises are flowed compound agitator, and it includes: be made up of three axial blades impeller of forming and three small front aprons 9 that are embedded in shaft end.
Impeller diameter d=0.5D
0(D
0Be the still diameter), impeller adopts the uniform pitch structure, blade from end of blade to the wide arc song (as Fig. 1) that is of root leaf, the center line of its any cross section is a camber line, the action of this camber line is 0.04-0.08 with the ratio of arc length, the leading edge of whole blade is repaiied the garden, and middle footpath is half (Fig. 2, Fig. 3) of vane thickness, and vane trailing edge is also accomplished circular arc.
Above-mentioned three rachises are flowed compound agitator 11 and are characterised in that: the laying angle of blade 10 end faces is 7-30 °, and the laying angle of root section is 40-110 °, and impeller is placed in high shaft end 0.5-0.7D
0The place, D
0Be pre-swelling still internal diameter, three baffle plates of shaft end 9 are uniform inlays welding, and the welding angle is 7-30 °, and direction is identical.Shaft end discharging opening plan range at the bottom of still is not more than 10mm.
Still Internal baffle 5 has four (see figure 5)s, and baffle plate and still wall spacing are D
0/ 60, baffle plate 5 length are D
0, the lower end is lower than impeller, impeller location 0.5D at the bottom of the still
0
Pre-swelling still by swelling kettle 1, oil lagging heat tracing layer 3, pipe by the kettle cover 12 of charge door, visor, air inlet/outlet and with at the bottom of the still, the baiting valve 8 of the controllable flow amount that is connected of charge door forms.
Connecting pipeline between the shunting guide pipe 7 that a special processing is housed between the charging aperture of baiting valve and measuring pump, this guider and measuring pump charging aperture does not have the dead angle.
Above-mentioned shunting guider also connects with the feed pipe 4 of kettle cover charging flange by another measuring pump.
Below kettle cover charging flange feed pipe, be a porous spray thrower 4.
Swelling equipment of this method and device parameter thereof are applicable to that volume is the pre-swelling still of 30L-50L.
In the method for the present invention, mix that high polymer content (weight) is 2%-50% in the preswollen even high polymer suspension, be preferably in 5%-20%.
It at room temperature is liquid that the solvent that uses requires, and is the good solvent decahydronaphthalene, makes fully swelling of high polymer like this, helps frozen glueization, for polyethylene, and the most handy decahydronaphthalene.
Swelling temperature is controlled at 30～100 ℃, and carrying out under the room temperature can also.
Swelling temperature is regulated by temperature in the control still, and it is monitored, regulates by the multichannel temperature controller by the hygrosensor 6 that inserts in the still.Swelling time is advisable to reach swelling equilibrium (Fig. 4), is no more than one hour at most, and from 10～60 minutes, when mixing pre-swelling, the rotating speed of agitator was controlled at 30-200r.p.m.
The rotating speed of agitator is low excessively, easily causes the sedimentation of powdery high polymer; Speed is too high, can cause whirlpool.Therefore, and select for use the apparatus structural parameters rationally to select for use according to material.
Above-mentioned through mixing preswollen heavy polymer unit for uniform suspension, as: powdery UHMWPE/ decahydronaphthalene (1%-2%) unit for uniform suspension continuously, is stably measured by measuring pump and is transported in the on-stream parallel dual-screw extruding machine, in 0.05D minute at most time, can in extruder, form the transparent frozen glue solution of homogeneous (D is a screw diameter, the mm of unit) fast.Material time of staying in extruder is no more than 10 minutes at most and promptly is extruded, the rotating speed of this double screw extruder is at 30-300r.P.m, the homogeneous frozen glue liquid that forms is extruded that machine is extruded after the filtration of the quick net exchanging device of head and pipeline that static mixer is housed are pressed to gear wheel metering pump, by measuring pump uniform frozen glue liquid is imported filament spinning component, and extrude, cool off the ecological gel fiber of formation through spinnerets, this gel fiber carries out the fiber that the super times hot-stretch of multistage makes high strength, high-modulus, low elongation after desolventizing, drying.
Embodiment and comparative example with the method for the invention is explained as follows below:
Embodiment
With powdery, weight average molecular weight is 3 * 10
6UHMW-PE and solvent decahydronaphthalene drop in the pre-swelling still of the present invention (open earlier stir and heating, after feed intake), polymer content 7wt%, feed intake and open bleeder valve after finishing and quantitatively be recycled into still in through the porous spray thrower material by shunting guider and measuring pump, after temperature reaches 100 ℃, proceed pre-swelling 20 minutes, make 7Wt% unit for uniform suspension (its suspension percentage is in 100 ± 0.5% scopes).
The parallel dual-screw that above-mentioned aaerosol solution another pilot hole by the shunting guider is transported to on-stream φ 35 through plunger metering pump with the 25ml/min volume flow is extruded the feed zone in district, and (extruder temperature is controlled at 160 ℃ except that feed zone, the screw rod revolution is 56rPm), just can continuously finish deaeration that suspension is converted into homogeneous frozen glue solution, frozen glue liquid in 5 minutes time, extrude, gained solution is transparent.Then extrude from spinnerets (32 holes, aperture 1mm) through spinning pump, assembly again, enter by the 150mm air column and solidify tank, get UHMW-PE frozen glue precursor with 2m/min speed seal wire.
With gained precursor desolventizing, drying, gained dry freeze glue fiber is with the speed of going into of 33cm/min, in the hot-stretch device of 120 ℃ and 145 ℃, stretch respectively, 35 times of total draw ratios can obtain intensity 30-35g/d, modulus 800-1200g/d and extend 3.0-3.5% high-strength, high-modulus polyethylene fiber.Spinning, stretching all can be continuous, stable, reach respectively more than 12 hours and 8 hours.
Among the embodiment, carry out tracking sampling to mixing pre-swelling system, come the stability of checking system discharge with the delivery time T of unit volume flow, with homogeneous, the stability of the weight of unit volume flow examination aaerosol solution solid content, and with auxiliary homogeneous, the stability that shows solid content of settling height.
See Table one, by survey the suspension percentage among the embodiment in 100 ± 0.5% scope.
Table one. the uniformity of the pre-swelling aaerosol solution of mixture and flow stability sampling sequence number amount of space sampling amount delivery time sample resedimentation height suspension percentage among the embodiment
| The sampling sequence number | Amount of space (ml) | Sampling amount (ml) | Delivery time (min) (sec) | Sample heavy (g) | Settling height (mm) | Suspension percentage % |
| 1 | 100 | 500 | 19 20 | 442．4 | 80 | 100．02 |
| 2 | 1500 | 500 | 19 31 | 442．9 | 80 | 100．13 |
| 3 | 1500 | 500 | 19 40 | 443．2 | 80 | 100．20 |
| 4 | 1500 | 500 | 19 54 | 444．2 | 80 | 100．43 |
| 5 | 1500 | 500 | 19 57 | 442．0 | 80 | 99．94 |
| 6 | 1500 | 500 | 19 57 | 439．9 | 80 | 99．46 |
| 7 | 500 | 500 | 19 59 | 441．6 | 80 | 99．85 |
In comparative example, material composition and content, swell process, spinning, desolventizing drying, drawing process technology are all identical.Owing to mix the different of pre-swelling equipment and technology, homogenizing stability to the mixture pre-swollen soln of powdery ultra-high molecular weight polyethylene has bigger influence, the delivery time fluctuation that shows the unit volume discharge is big, the sample of unit volume discharge heavily fluctuates greatly, and settling height is also unstable.
The same embodiment of comparative example 1 process implementing, but do not adopt shunting guiding circulation measure, suspension system homogenizing is poor than embodiment, and is as shown in table 2, and its suspension percentage is in 100 ± 0.8% scopes, and the circulation of visible shunting guiding helps improving even suspension percentage.Though can extrude homogeneous jelly solution and continuous extruding spinning from screw rod, the fiber number of gel fiber is influenced not quite basically.Table 2 does not have uniformity and the flow stability that the circulation of shunting guiding mixes pre-swollen soln
| The sampling sequence number | Amount of space (ml) | Sampling amount (ml) | Delivery time (min) (sec) | Sample heavy (g) | Settling height (mm) | Suspension percentage % |
| 1 | 500 | 500 | 20 27 | 442 | 95 | 99．8 |
| 2 | 2000 | 500 | 20 16 | 446．2 | 93 | 100．74 |
| 3 | 1500 | 500 | 20 16 | 443．8 | 90 | 100．2 |
| 4 | 1500 | 500 | 20 22 | 443．2 | 75 | 100．06 |
| 5 | 1500 | 500 | 20 17 | 442．3 | 70 | 99．87 |
| 6 | 1500 | 500 | 20 05 | 440．0 | 50 | 99．35 |
| 7 | 1200 | 500 | 20 00 | ／ | ／ |
The same embodiment of comparative example 2 process implementings, but mix in the pre-swelling still and do not add baffle plate, do not adopt shunting guiding circulation measure yet, even suspension percentage and stable results measured to this suspension mixed system are listed in table 3, as shown in Table 3, the axial uniformity deviation of the pre-swelling suspension of unbaffled mixing is bigger, overgauge+0.73%, minus deviation-1.12% promptly has sedimentation trend to exist.Uniformity and flow stability that no baffle plate of table 3. and the circulation of shunting guiding mix pre-swelling suspension
| The sampling sequence number | Amount of space (ml) | Sampling amount (ml) | Delivery time (min) (sec) | Sample heavy (g) | Settling height (mm) | Suspension percentage % |
| 1 | 3250 | 500 | 19 59 | 446 | 100 | 100．73 |
| 2 | 3250 | 500 | 19 56 | 445．6 | 93 | 100．64 |
| 3 | 6500 | 500 | 20 46 | 441．6 | 90 | 99．74 |
| 4 | 3250 | 500 | 20 58 | 437．8 | 68 | 98．88 |
Comparative example 3-5 illustrates (table 4) with the influence that the gel spun fiber fiber number is changed
Table 4. mixes the influence of pre-swelling mode to gel spun fiber fiber number stability and spinnability
| Embodiment | Mix pre-swelling mode | Gel spun fiber fiber number (ten thousand dawn) wire vent 30 minutes 150 minutes 270 minutes 390 minutes 630 minutes | |||||
| Embodiment 1 | 1 *+2 **+3 *** | 21．14 | 21．14 | 21．13 | 21．13 | 21．13 | |
| Comparative example 1 | 1 *+2 ** | 21．13 | 21．33 | 21．1 | 20．93 | 20．03 | |
| Comparative example 2 | 1 * | 21．16 | 21．5 | 21．2 | 19．45 | 19 | |
| Comparative example 3 | Three vane types | 20 | 19 | 11．5 | 10．0 | ／ | |
| Comparative example 4 | The anchor formula | ／ | ／ | ／ | ／ | ／ | |
| Comparative example 5 | Two helical-ribbon types | ／ | ／ | ／ | ／ | ／ | |
Four baffle plates in the pre-swelling still of *
* * shunting guiding circulated sprinkling system
"/" expression spinnability is poor
Claims (10)
1. the continuous preparation method of superhigh molecular weight polyethylene fibers is characterized in that described preparation method is as follows:
Powdery ultra-high molecular weight polyethylene and whole solvents of being mixed with finite concentration frozen glue solution are by weight dropped into together carry out swelling in the pre-swelling still and all mix, make the unit for uniform suspension of heavy polymer;
Above-mentioned through mix preswollen super high molecular weight polymer unit for uniform suspension by measuring pump continuously, metering stably is transported in the on-stream parallel dual-screw extruding machine, can form the transparent frozen glue solution of homogeneous fast in 0.05D minute at most time in extruder.Wherein, D is a screw diameter, and unit is mm.
Material time of staying in extruder is no more than 10 minutes at most and promptly is extruded, and the rotating speed of this double screw extruder is at 30-300rpm;
The homogeneous frozen glue solution that forms is extruded that machine is extruded after the filtration of the quick net exchanging device of head and pipeline that static mixer is housed are pressed to gear wheel metering pump, by measuring pump uniform frozen glue liquid is imported filament spinning component, and extrude, cool off the ecological gel fiber of formation through spinnerets; This gel fiber carries out the super times thermal potential of multistage and stretches the fiber that makes high strength, high-modulus, low elongation after desolventizing, drying.
Described solvent is a decahydronaphthalene.
2. method according to claim 1 is characterized in that described method is applicable to that volume is the pre-swelling still of 30L-50L.
3. method according to claim 1 is characterized in that high polymer content (weight) is 2%～50% in the preswollen even high polymer suspension of described mixing.
4. method according to claim 1 is characterized in that high polymer content (weight) is preferably in 5%-20% in the pre-broad bloated even high polymer suspension of described mixing.
5. method according to claim 1 is characterized in that described swelling temperature at 30-100 ℃, and carrying out under the room temperature can also.
6. method according to claim 1 is characterized in that described swelling time is advisable to reach swelling equilibrium, is no more than one hour at most, and from 10-60 minutes, when mixing pre-swelling, the rotating speed of agitator was controlled at 30-200r.P.m.
7. an equipment that is used for the continuous preparation method of superhigh molecular weight polyethylene fibers comprises pre-swelling still, shunting guider, double screw extruder, it is characterized in that described pre-swelling still comprises: kettle (1), oil lagging (2), heat-insulation layer (3), porous spray thrower (4), baffle plate (5), temperature tube (6), shunting guider (7), bleeder valve (8), axle head baffle plate (9), CBY axial blade (10), CBY three rachises are flowed compound agitator (11), kettle cover (12).
Concrete is that CBY type three rachises are flowed compound agitator, and it includes: form by three axial blades impeller of forming and three small front aprons (9) that are embedded in shaft end,
Impeller diameter d=0.5D
0, D
0Be the still diameter, impeller adopts the uniform pitch structure, blade from end of blade to the wide arc song that is of root leaf, the center line of its any cross section is a camber line, the action of this camber line is 0.04-0.08 with the ratio of arc length, and the leading edge of whole blade is repaiied the garden, and middle footpath is half of vane thickness, vane trailing edge is also accomplished circular arc
Above-mentioned three rachises are flowed compound agitator (11) and are characterised in that: the laying angle of blade (10) end face is 7-30 °, and the laying angle of root section is 40-110 °, and impeller is placed in high shaft end 0.5-0.7D
0The place, D
0Be pre-swelling still internal diameter, three baffle plates of shaft end (9) are uniform inlays welding, and the welding angle is 7-30 °, and direction is identical.Shaft end discharging opening plan range at the bottom of still is not more than 10mm,
Still Internal baffle (5) has four, and baffle plate and still wall spacing are D
0/ 60, baffle plate (5) length equals D
0, the lower end is lower than impeller, impeller location 0.5D at the bottom of the still
0,
Pre-swelling still by swelling kettle (1), oil lagging (2) heat tracing layer (3), pipe have charge door, visor, air inlet/outlet kettle cover (12) and with at the bottom of the still, the baiting valve (8) of the controllable flow amount that is connected of charge door forms,
There is not the dead angle at the connecting pipeline that is equipped with between the charging aperture of baiting valve and measuring pump between shunting guide pipe (7), this guider and the measuring pump charging aperture of a special processing,
Above-mentioned shunting guider also connects with the feed pipe (4) of kettle cover charging flange by another measuring pump,
Below kettle cover charging flange feed pipe, be a porous spray thrower (4).
8. equipment according to claim 7 is characterized in that: described β a is the root of blade laying angle, and β t is the vane end faces laying angle, and the laying angle β i from the impeller center to arbitrary cross section, end of blade different radii place presses the uniform pitch structural design.
9. according to claim 7 or 8 described equipment, it is characterized in that described blade from end face (13) to root (14) along leaf the wide cambered surface that is, the center line of cross section (15) is a camber line arbitrarily, the radius of curvature R of this section determines that with the ratio of arc length a its ratio is in 0.04-0.08 scope by the action h of center camber line on this cross section.
10. the continuous preparation method's of superhigh molecular weight polyethylene fibers according to claim 7 equipment is characterized in that described whole blade leading edge (16) repaiies the garden, and radius r is half of vane thickness, and trailing edge (17) is also accomplished transition arc.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97101010A CN1060543C (en) | 1997-01-02 | 1997-01-02 | Method and apparatus for continuous making superhigh molecula polyethylene fibre |
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|---|---|---|---|
| CN97101010A CN1060543C (en) | 1997-01-02 | 1997-01-02 | Method and apparatus for continuous making superhigh molecula polyethylene fibre |
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| CN1060543C true CN1060543C (en) | 2001-01-10 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0167187A1 (en) * | 1984-05-11 | 1986-01-08 | Stamicarbon B.V. | Novel irradiated polyethylene filaments, tapes and films and process therefor |
| CN1050884A (en) * | 1989-10-13 | 1991-04-24 | 中国纺织大学 | The preparation of extra-high molecular weight polythene uniform solution |
| CN2173792Y (en) * | 1993-11-20 | 1994-08-10 | 中国人民解放军总后勤部军需装备研究所 | Apparatus for preparing spinning solution of superhighmolecular polyethylene |
-
1997
- 1997-01-02 CN CN97101010A patent/CN1060543C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0167187A1 (en) * | 1984-05-11 | 1986-01-08 | Stamicarbon B.V. | Novel irradiated polyethylene filaments, tapes and films and process therefor |
| CN1050884A (en) * | 1989-10-13 | 1991-04-24 | 中国纺织大学 | The preparation of extra-high molecular weight polythene uniform solution |
| CN2173792Y (en) * | 1993-11-20 | 1994-08-10 | 中国人民解放军总后勤部军需装备研究所 | Apparatus for preparing spinning solution of superhighmolecular polyethylene |
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|---|---|
| CN1160093A (en) | 1997-09-24 |
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