CN102277632B - Method for manufacturing gel-spun ultra-high molecular weight polyethylene fiber - Google Patents
Method for manufacturing gel-spun ultra-high molecular weight polyethylene fiber Download PDFInfo
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Abstract
The invention discloses a method for manufacturing gel-spun ultra-high molecular weight polyethylene fibers. The method comprises the following steps of: primarily treating ultra-high molecular weight polyethylene powders and solvents with a double screw extruder under a certain condition to obtain an extrusion liquid; further treating the extrusion liquid with the double screw extruder under a certain condition to obtain extruded materials; and carrying out spinning treatment, static balance treatment, extraction treatment, primary drawing treatment and ultra-drawing treatment and the like on the extruded materials under a certain condition, to obtain gel-spun ultra-high molecular weight polyethylene fibers. By using the method, the technical problem in the prior art that ultrahigh temperature and ultrahigh shearing force are applied to achieve ultrahigh orientation of molecular chains, resulting in severe degradation of molecular chains and low screw efficiency can be solved; the spinning property of fiber spinning flows is greatly improved; molecular orientation property of fiber spinning flows is improved; and the strength and toughness of fiber spinning flows are increased.
Description
Technical field
The present invention relates to the manufacture method of polyethylene fiber gel spinning, relate in particular to a kind of method of making the superhigh molecular weight polyethylene fibers gel spinning.
Background technology
The manufacturing of relevant superhigh intensity high-modulus superhigh molecular weight polyethylene fibers, industry up to now both at home and abroad, basically still after using ultra-high molecular weight polyethylene powder and solvent blend, enter fusion in the double screw extruder-dissolving extruding spinning thread, form fiber through super times hot-stretch again.And preparation quality homogeneous, the big good spinning solution of molecular assembly are prerequisite and the basis of preparation high-strength high-modulus polyethylene fiber.Adopt single double screw extrusion method at present, Polymer Solution has experienced short time high temperature, big shear history in screw rod, and ultra-high molecular weight polyethylene tangible signs of degradation will occur above under 260 ℃ the high temperature, can bring negative influence to the spinnability of spinning solution after degrading, bring the negative influence of spinnability because of macromolecules degradation for the extrusion solution thread, thereby reduce the performance of finished fiber.
This shows that prior art needs further improvement and develops.
Summary of the invention
The present invention provides a kind of method of making the superhigh molecular weight polyethylene fibers gel spinning for solving above-mentioned defective of the prior art, solution is the too high technical problem that causes the ultra-high molecular weight polyethylene degraded of temperature in making superelevation polyethylene fiber gel spinning process, to improve its molecularly oriented, strengthen its strength and toughness.
For solving the problems of the technologies described above, the present invention program comprises:
A kind of method of making the superhigh molecular weight polyethylene fibers gel spinning, it may further comprise the steps:
A, with mass fraction between 6%～12%, to be 1,500,000-1,000 ten thousand ultrahigh molecular weight polyethylene powder with solvent delivery fully mix in the batching emulsification still viscosity average molecular weigh obtains mixture, this mixture enters the feeding still through the gear delivery pump, the feeding still is sent mixture into double screw extruder and is carried out fusion-dissolving, obtains extruding liquid;
B, the above-mentioned liquid of extruding are compressed into into single screw extrusion machine through the coarse filter band, single screw diameter is 20mm-150mm in this single screw extrusion machine, its draw ratio is 20-25, its rotating speed is 70 rev/mins-140 rev/mins, this single screw extrusion machine is by three sections heating, feeding section temperature at 180 ℃-220 ℃, fluxing zone temperature at 200 ℃-240 ℃, homogenizing zone temperature at 220 ℃-260 ℃, the highest extrusion temperature of this single screw extrusion machine is 240 ℃; The above-mentioned liquid of extruding obtains extruded material through the single screw extrusion machine processing;
C, above-mentioned extruded material is delivered to spinnerets by the melt booster pump by fine filter, spinnerets is extruded the extruded material metering and is flooded in chilled water and obtains the gel spun, with extract behind this gel spun static balance, 5 times of-10 times of preliminary stretch processings, and then under multistage ladder-elevating temperature condition, carry out 3 times of-8 times of ultra-drawing orientation process, obtain the superhigh molecular weight polyethylene fibers gel spinning.
Described manufacture method, wherein, above-mentioned steps A comprises that also the twin-screw diameter of described double screw extruder is between 28mm-340mm, the draw ratio of twin-screw is 7-18, the temperature of each of twin-screw section is at 140 ℃-260 ℃, the rotating speed of twin-screw is 180 rev/mins-250 rev/mins, and the highest extrusion temperature of double screw extruder is 260 ℃.
Described manufacture method, wherein, the aperture of above-mentioned spinnerets is 0.5mm-1mm, and hole count is holes, 100 holes-150, and spray silk speed is 4 meters/minute-10 meters/minute.
Described manufacture method, wherein, above-mentioned steps C comprises that also the temperature of above-mentioned chilled water is 10 ℃-15 ℃, and the time of gel spun static balance is 20 hours-30 hours, and the temperature of multistage ladder-elevating temperature is 80 ℃-150 ℃.
Described manufacture method, wherein, the above-mentioned orientation index that obtains the superhigh molecular weight polyethylene fibers gel spinning is 95-97, and fracture strength is 30cN/dtex-50cN/dtex, and modulus is 1200/dtex～1400/dtex.
A kind of method of making the superhigh molecular weight polyethylene fibers gel spinning provided by the invention, ultra-high molecular weight polyethylene is handled by double screw extruder under certain condition, then it is being handled through single screw extrusion machine under certain condition, namely finished super high molecular polyethylene solution under the low shearing condition of low temperature, further dissolving, homogenize has also improved the process of superhigh molecular weight polyethylene fibers order, for spinning provides quality higher solution thread, solved in the existing superhigh molecular weight polyethylene fibers gel spinning technical process, used the too high shearing force of high temperature for making strand superelevation orientation, thereby cause the strand severely degrade, the inefficient technical problem of screw rod, make spinning temperature by original 280 ℃-290 ℃, be reduced to 240 ℃-260 ℃, the viscosity average molecular weigh of extruding liquid is 3,200,000, and the viscosity average molecular weigh of extruding liquid of the prior art is 2,600,000, the viscosity average molecular weigh of extruding liquid among the present invention is compared with prior art and has been improved 23%, the maximum spinning head draw ratio of fiber is of the prior art to have increased by one times, improved the spinnability of fiber thread greatly, improve its molecularly oriented, strengthened its strength and toughness.
Description of drawings
Fig. 1 is the schematic flow sheet of making the superhigh molecular weight polyethylene fibers gel spinning among the present invention.
The specific embodiment
The invention provides a kind of method of making the superhigh molecular weight polyethylene fibers gel spinning, clearer, clear and definite in order to make purpose of the present invention, technical scheme and advantage, below with reference to accompanying drawing and embodiment, the present invention is described in more detail.
The invention provides a kind of method of making the superhigh molecular weight polyethylene fibers gel spinning, ultra-high molecular weight polyethylene is handled through double screw extruder and single screw extrusion machine successively, ultra high molecular polyethylene is handled under the low shearing condition of low temperature, prevented that ultra-high molecular weight polyethylene from signs of degradation taking place in processing procedure, improve its molecularly oriented, strengthened its strength and toughness.Its concrete technology mainly comprises as shown in Figure 1:
Step a: with mass fraction between 6%～12%, to be 1,500,000-1,000 ten thousand ultrahigh molecular weight polyethylene powder with solvent delivery fully mix in the batching emulsification still viscosity average molecular weigh obtains mixture, wherein, solvent generally adopts White Mineral Oil, paraffin oil or its mixture; This mixture enters the feeding still through the gear delivery pump, and the feeding still is sent mixture into double screw extruder and carried out fusion-dissolving, obtains extruding liquid;
Step b: the above-mentioned liquid of extruding is compressed into into single screw extrusion machine through the coarse filter band, single screw diameter is 20mm-150mm in this single screw extrusion machine, its draw ratio is 20-25, its rotating speed is 70 rev/mins-140 rev/mins, this single screw extrusion machine is by three sections heating, feeding section temperature at 180 ℃-220 ℃, fluxing zone temperature at 200 ℃-240 ℃, homogenizing zone temperature at 220 ℃-260 ℃, the highest extrusion temperature of this single screw extrusion machine is 240 ℃; The above-mentioned liquid of extruding obtains extruded material through the single screw extrusion machine processing; Extrude liquid under certain condition after step a handled, extrude through single screw extrusion machine again, under 260 ℃ of conditions, make extruded material, avoided ultra-high molecular weight polyethylene that signs of degradation takes place in processing procedure, improved the combination property of extruded material.
Step c: above-mentioned extruded material is delivered to spinnerets by the melt booster pump by fine filter, spinnerets is extruded the extruded material metering and is flooded in chilled water and obtains the gel spun, with extract behind this gel spun static balance, 5 times of-10 times of preliminary stretch processings, and then under multistage ladder-elevating temperature condition, carry out 3 times of-8 times of ultra-drawing orientation process, obtain the superhigh molecular weight polyethylene fibers gel spinning.
In order further to improve performance of the present invention, step a comprises that also the twin-screw diameter of described double screw extruder is between 28mm-340mm, the draw ratio of twin-screw is 7-18, the temperature of each of twin-screw section is at 140 ℃-260 ℃, the rotating speed of twin-screw is 180 rev/mins-250 rev/mins, the highest extrusion temperature of double screw extruder is 260 ℃, ultra-high molecular weight polyethylene is carried out preliminary treatment under certain condition, for subsequent step provides the stable liquid of extruding.
Further, the aperture of spinnerets is 0.5mm-1mm, and hole count is holes, 100 holes-150, and spray silk speed is 4 meters/minute-10 meters/minute, makes the superhigh molecular weight polyethylene fibers gel spinning more even.
Further, the temperature of above-mentioned chilled water is 10 ℃-15 ℃, and the time of gel spun static balance is 20 hours-30 hours, and the temperature of multistage ladder-elevating temperature is 80 ℃-150 ℃, make the superhigh molecular weight polyethylene fibers gel spinning have the macromolecular orientation degree, mechanical property is better.
The orientation index of the superhigh molecular weight polyethylene fibers gel spinning that obtains by technology of the present invention is 95-97, and fracture strength is 30cN/dtex-50cN/dtex, and modulus is 1200/dtex～1400/dtex, is improved largely in prior art.
In order further to describe, then with mass fraction between 6～12%, viscosity average molecular weigh is that 1,500,000-1,000 ten thousand ultrahigh molecular weight polyethylene powder and solvent fully mix and obtain mixture, the mass ratio of ultrahigh molecular weight polyethylene powder and solvent is 1: 2-15, this mixture is transported in the batching emulsification still by the automatic gauge mode, in the gear delivery pump enters the feeding still, in double screw extruder, finish preliminary fusion-dissolving and obtain extruding liquid, the twin-screw diameter of double screw extruder is between 28mm-340mm, screw slenderness ratio is between 7-18, the screw zones temperature is between 140 ℃-260 ℃, the extruded velocity of screw rod is at 180 rev/mins-250 rev/mins, the outlet temperature of double screw extruder is the highest to be set at 260 ℃, extrude liquid through behind the coarse filter, band is compressed into single screw extrusion machine, single screw diameter is between 20mm-150mm, single screw slenderness ratio of single screw extrusion machine is between 20-25, single screw speed is between 70 rev/mins-140 rev/mins, material is further dissolving in single screw extrusion machine, homogenize, and constant temperature is extruded and is obtained extruded material, the heating hop count of single screw extrusion machine is three sections, be that feeding section temperature is at 180 ℃-220 ℃, the fluxing zone temperature is at 200 ℃-240 ℃, the homogenizing zone temperature is at 220 ℃-260 ℃), the highest extrusion temperature is set at 240 ℃, after extruded material passes through fine filter by the melt booster pump again, extruded in the spinnerets metering of 0.5mm-1.0mm hole count between the 100-150 hole by the aperture; Chilled water dipping at 10 ℃-15 ℃ is the gel spun, and 4 meters/minute-10 meters/minute of the spray silk speed of spinnerets are received the collection of gel spun with institute and left standstill balance 20 hours-30 hours; Gel spun behind the static balance is after extraction, 5-10 stretch at the beginning of doubly, again through multistage ladder-elevating temperature { 80 ℃～150 ℃ } draw ratio 3-8 times of ultra-drawing orientation process, obtaining orientation index is 95～97, and fracture strength is that 30cN/dtex～50cN/dtex, modulus are the superelevation superhigh molecular weight polyethylene fibers gel spinning of 1200/dtex～1400/dtex.
Certainly, above-mentioned explanation is not to be limitation of the present invention, and the present invention also is not limited in above-mentioned giving an example, and the variation that those skilled in the art make in essential scope of the present invention, remodeling, interpolation or replacement also should belong to protection scope of the present invention.
Claims (2)
1. method of making the superhigh molecular weight polyethylene fibers gel spinning, it may further comprise the steps:
A, with mass fraction between 6%～12%, to be 1,500,000-1,000 ten thousand ultrahigh molecular weight polyethylene powder with solvent delivery fully mix in the batching emulsification still viscosity average molecular weigh obtains mixture, this mixture enters the feeding still through the gear delivery pump, the feeding still send double screw extruder to carry out fusion-dissolving in mixture, obtains extruding liquid;
B, the above-mentioned liquid of extruding are compressed into into single screw extrusion machine through the coarse filter band, single screw diameter is 20mm-150mm in this single screw extrusion machine, its draw ratio is 20-25, its rotating speed is 70 rev/mins-140 rev/mins, this single screw extrusion machine is by three sections heating, feeding section temperature at 180 ℃-220 ℃, fluxing zone temperature at 200 ℃-240 ℃, homogenizing zone temperature at 220 ℃-260 ℃, the highest extrusion temperature of this single screw extrusion machine is 240 ℃; The above-mentioned liquid of extruding obtains extruded material through the single screw extrusion machine processing;
C, above-mentioned extruded material is delivered to spinnerets by the melt booster pump by fine filter, spinnerets is extruded the extruded material metering and is flooded in chilled water and obtains the gel spun, with extract behind this gel spun static balance, 5 times of-10 times of preliminary stretch processings, and then under multistage ladder-elevating temperature condition, carry out 3 times of-8 times of ultra-drawing orientation process, obtain the superhigh molecular weight polyethylene fibers gel spinning;
Above-mentioned steps A comprises that also the twin-screw diameter of described double screw extruder is between 28mm-340mm, the draw ratio of twin-screw is 7-18, the temperature of each of twin-screw section is at 140 ℃-260 ℃, the rotating speed of twin-screw is 180 rev/mins-250 rev/mins, and the highest extrusion temperature of double screw extruder is 260 ℃;
Above-mentioned steps C comprises that also the temperature of above-mentioned chilled water is 10 ℃-15 ℃, and the time of gel spun static balance is 20 hours-30 hours, and the temperature of multistage ladder-elevating temperature is 80 ℃-150 ℃;
The above-mentioned orientation index that obtains the superhigh molecular weight polyethylene fibers gel spinning is 95-97, and fracture strength is 30cN/dtex-50cN/dtex, and modulus is 1200/dtex～1400/dtex.
2. manufacture method according to claim 1, it is characterized in that: the aperture of above-mentioned spinnerets is 0.5mm-1mm, and hole count is holes, 100 holes-150, and spray silk speed is 4 meters/minute-10 meters/minute.
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| CN111118615A (en) * | 2019-12-26 | 2020-05-08 | 长青藤高性能纤维材料有限公司 | Method for treating spinning dope of ultra-high molecular weight polyethylene fiber |
| CN115595684A (en) * | 2022-02-14 | 2023-01-13 | 江苏锵尼玛新材料股份有限公司（Cn） | Preparation and application of efficient green pollution-free ultra-high molecular weight polyethylene fiber |
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| CN1190137A (en) * | 1997-12-10 | 1998-08-12 | 中国纺织大学 | Continuous preparation of homogeneous solution of superhigh molecular weight polythene |
| CN1432077A (en) * | 2000-03-27 | 2003-07-23 | 霍尼韦尔国际公司 | High tenacity, high modulus filament |
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| CN101781808A (en) * | 2009-01-15 | 2010-07-21 | 上海博迪纺织新材料有限公司 | Device for two-stage continuous dissolution, untwisting and spinning of homogeneous solution of ultra-high molecular weight polyethylene |
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| JPS6173743A (en) * | 1984-09-20 | 1986-04-15 | Kuraray Co Ltd | Method for continuously preparing stock solution of high-molecular polyolefin |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1190137A (en) * | 1997-12-10 | 1998-08-12 | 中国纺织大学 | Continuous preparation of homogeneous solution of superhigh molecular weight polythene |
| CN1432077A (en) * | 2000-03-27 | 2003-07-23 | 霍尼韦尔国际公司 | High tenacity, high modulus filament |
| CN101781808A (en) * | 2009-01-15 | 2010-07-21 | 上海博迪纺织新材料有限公司 | Device for two-stage continuous dissolution, untwisting and spinning of homogeneous solution of ultra-high molecular weight polyethylene |
| CN101724921A (en) * | 2009-11-26 | 2010-06-09 | 宁波大成新材料股份有限公司 | Process for evenly preparing spinning by using ultrahigh molecular weight polyethylene high-shearing solution |
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Effective date of registration: 20160912 Address after: 266510 Shandong, Qingdao Province, No. six road, Huangdao District No. 16 Patentee after: QINGDAO ZHONGKE HUALIAN NEW MATERIAL CO., LTD. Address before: Six 16 mountain road, 266555 economic and Technological Development Zone, Shandong, Qingdao Patentee before: Qingdao Huashijie Environment Protection Technology Co., Ltd. |