CN102199798B - Preparation method of ultrahigh-molecular-weight polyethylene fine denier fibers - Google Patents
Preparation method of ultrahigh-molecular-weight polyethylene fine denier fibers Download PDFInfo
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- CN102199798B CN102199798B CN 201110090624 CN201110090624A CN102199798B CN 102199798 B CN102199798 B CN 102199798B CN 201110090624 CN201110090624 CN 201110090624 CN 201110090624 A CN201110090624 A CN 201110090624A CN 102199798 B CN102199798 B CN 102199798B
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Abstract
The invention relates to a method for preparing ultrahigh-molecular-weight polyethylene fine denier fibers by a jelly spinning process, which comprises: (1) preparing jelly protofilaments of ultrahigh-molecular-weight polyethylene; and (2) subjecting the jelly protofilaments to pre-stretching, extraction, drying and hot stretching to obtain ultrahigh-molecular-weight polyethylene fine denier fibers, wherein the pre-stretching is performed for many times till the jelly protofilaments are stretched by 15 to 35 times totally, the many times of stretching are all performed in a stretching medium at 30 to 50 DEG C, the stretching medium is air, water or oil, and the jelly protofilaments are hotly stretched by 35 to 50 times totally. And after the step (1) and before the step (2), the method also comprises a step of standing the jelly protofilaments at a constant temperature of 20 to 40 DEG C and a constant humidity of 30 to 60 percent for 48 to 72 hours. When the method is used, low-titre and high-breaking-strength ultrahigh-molecular-weight polyethylene fine denier fiber products can be obtained, and the production cost is low.
Description
Technical field
The present invention relates to a kind of preparation method of ultrahigh-molecular-weight polyethylene fine denier fibers.
Background technology
Superhigh molecular weight polyethylene fibers (UHMWPE) is a kind of high-performance fiber of succeeding in developing and entering the beginning of the eighties industrialization end of the seventies in last century, with carbon fiber, aramid fiber and be called the world today's three large tec fibers, mainly at present produce by the gel spinning method.In the prior art, the key step of gel spinning method is as follows: extruded by screw extruder by the stoste that ultra-high molecular weight polyethylene powder and suitable solvent are made into, the spinneret orifice moulding, enter water-bath and solidify the frozen glue precursor that obtains polyethylene fiber, this frozen glue precursor is through extraction, and drying obtains finished fiber after the super times hot-stretch, wherein, obtain low-titer or the little fiber of dawn number by improving the jet stretch multiplying power.The weak point of the method is, the ultra-drawing multiplying power is crossed the structure that conference destroys gel spun fiber, causes drawing-off irregular, so that finished fiber easily ruptures.
Publication number is the preparation method that the Chinese invention patent application of CN 101768786A discloses a kind of superhigh molecular weight polyethylene fibers, wherein disclosed before extraction, it is 2.2～24 times preliminary draft that the frozen glue precursor is carried out multiple, can reduce the amount of the solvent in the frozen glue precursor by preliminary draft, the frozen glue precursor is attenuated, so, when the hot-stretch of rear road, only need under low multiple, can obtain the polyethylene fiber of low-titer.Simultaneously, because the multiple of hot-stretch is lower, thereby can not destroys the structure of gel spun fiber and fall low-fiber fracture strength.In addition, quantity of solvent reduces in the frozen glue precursor because preliminary draft makes, and follow-up extraction and drying process can more easily and faster carry out, and the consumption of extractant reduces.As seen, preliminary draft is for improving the stable significant of extraction efficiency and postchannel process.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of improved ultrahigh-molecular-weight polyethylene fine denier fibers, further improves the extraction efficiency in the fiber preparation process, technology stability and fall low-fiber irregularity.
For solving above technical problem, the present invention takes following technical scheme:
The method of the standby ultrahigh-molecular-weight polyethylene fine denier fibers of a kind of gel spinning legal system, it comprises the frozen glue precursor of (1), preparation ultra-high molecular weight polyethylene; (2), the frozen glue precursor is successively through preliminary draft, extraction, drying and hot-stretch obtain described high molecular weight polyethylene fiber, wherein: described preliminary draft carries out repeatedly altogether, and repeatedly the general times of preliminary draft is 15～35 times, repeatedly preliminary draft all carries out in 30 ℃～50 ℃ drawing-off medium, described drawing-off medium is air, water or oil, the general times of described hot-stretch is 35～50 times, described method also is included in step (1) afterwards, step (2) is 20 ℃～40 ℃ with described frozen glue precursor in temperature before, humidity is to leave standstill 48～72 hours under 30%～60% the constant temperature and humidity condition.
Preferably, described drawing-off medium is 30 ℃～40 ℃ air.Described preliminary draft preferably carries out 2～4 times altogether, and most preferably 3 times, and drafting multiple reduces one by one, and last pre-draft multiple is 1.1～1.5.
Preferably, in the step (2), the agent for carbon hydrogen detergent that the alkane of described extraction employing boiling point between 125 ℃～155 ℃ for example can directly be bought from the market is as extractant.
Said method can obtain fracture strength more than 35cn/dtex according to the present invention, and modulus is more than 1200 g/d, and denier irregularity is lower than ± 2% ultrahigh-molecular-weight polyethylene fine denier fibers, and the total denier of fiber is preferably 30～400D.
Because the enforcement of above technical scheme, the present invention compared with prior art has following advantage:
The inventive method is optimized preliminary draft technique, the one, keep a period of time before the preliminary draft frozen glue precursor being placed under the specific temperature and humidity condition, in the process of leaving standstill, the frozen glue precursor is contracted to original 0.4～0.5 times, shrink more even, so that follow-up preliminary draft can carry out by larger multiple, and more steady; The 2nd,, preliminary draft is carried out several times, compared with the prior art the preliminary draft general times significantly improves, and repeatedly preliminary draft all carries out in specific drawing-off medium, so, and on the one hand, thinner through the gel spun fiber behind the preliminary draft, follow-up extraction efficiency is higher, and solvent is more saved, and greatly reduces the fiber number of finished fiber; On the other hand, the intensity of the gel fiber behind the process preliminary draft obviously increases, and makes postchannel process more stable, more is not prone to the situations such as lousiness, broken end, has reduced simultaneously the irregularity of finished fiber fiber number.
The specific embodiment
Embodiment 1
Preparation method according to the superhigh molecular weight polyethylene fibers of the present embodiment comprises the steps:
(1), the frozen glue precursor of preparation ultra-high molecular weight polyethylene: with ultra-high molecular weight polyethylene (relative average molecular mass 4,500,000); dissolvant white oil 70# and phenol type antioxidant; 8:100:0.16 is injected into respectively solution and twines in the still in mass ratio; nitrogen protection down cut 25 minutes, shear rate 3000 seconds
-1
, obtain the mixed liquor of emulsion form, then this mixed liquor is input to and carries out second in the high cut disperse emulsification pump and shear, out the part of mixed liquor is fed in the screw extruder from emulsification pump, and remainder loops back solution and twines in the still.In this example, screw extruder is twin-screw, screw extruder diameter 95mm, length-to-diameter is 64,285 ℃ of the temperature of screw rod, rotating speed 160 rpm, the extrudate of screw extruder output pass through behind filter, casing, the measuring pump successively from spinneret orifice (diameter 0.7mm) ejection of spinning pack, then enter in the water-bath that contains the 1wt% surfactant under 20 ℃ and solidify.Adjustment by technological parameters such as measuring pump, spinneret drafts, obtain respectively the frozen glue precursor of 100D, 200D, 400D, afterwards the frozen glue precursor that obtains is placed (25 ℃ of constant temperature and humidity conditions, humidity 50%) under, static depositing more than 48 hours is controlled between 40%～50% the relaxation shrinkage of frozen glue precursor.
(2), step (1) gained 400D frozen glue precursor is carried out preliminary draft altogether three times, wherein, the multiple of three preliminary drafts is followed successively by 4 times, and 3.5 times and 1.2 times, total pre-draft multiple is 16.8 times, and in the preliminary draft process, below every group of drawing roller of its process section, pass to 35 ℃ of hot-airs of constant flow, along with the continuous refinement of gel spun fiber, the gel spun fiber radical that drawing roller can be arranged has improved 20% than original technique, also is that output has increased by 20%.
(3), take agent for carbon hydrogen detergent as extractant, the frozen glue precursor through step (2) is extracted, afterwards, drying obtains total denier 400D, the superhigh molecular weight polyethylene fibers of filament number 1.2D through 35 times hot-stretchs.After testing, fibrous fracture intensity surpasses 37cn/dtex, and modulus is more than 1200 g/d, and the denier irregularity of fiber is lower than ± 2%.
Embodiment 2
Preparation method according to the superhigh molecular weight polyethylene fibers of the present embodiment comprises the steps:
(1), with embodiment 1;
(2), step (1) gained 100D frozen glue precursor is carried out preliminary draft altogether three times, wherein, the multiple of three preliminary drafts is followed successively by 5.5 times, 3.5 doubly with 1.1 times, its general times is 21.2 times, in this process, every group of drawing roller of preliminary draft process section places 35 ℃ hydrocarbon class finish, this finish supply is certain, and passes to outer circulation, fully guarantees the stability of its concentration and temperature.And, after this finish uses, can carry out subsequent recovery.The gel spun fiber radical that drawing roller can be arranged has improved 30% than original technique, also is that output has increased by 30%.
(3), take agent for carbon hydrogen detergent as extractant, the frozen glue precursor through step (2) is extracted, afterwards, drying obtains total denier 100D, the superhigh molecular weight polyethylene fibers of filament number 1 D through 40 times hot-stretchs.After testing, fibrous fracture intensity surpasses 40cn/dtex, and modulus is more than 1300 g/d, and the denier irregularity of fiber is lower than ± 2%.
Comparative Examples 1
Preparation method according to the superhigh molecular weight polyethylene fibers of this Comparative Examples comprises the steps:
(1), the frozen glue precursor of preparation ultra-high molecular weight polyethylene: with ultra-high molecular weight polyethylene (relative average molecular mass 4,500,000); dissolvant white oil 70# and phenol type antioxidant; 8:100:0.16 is injected into respectively solution and twines in the still in mass ratio; nitrogen protection down cut 25 minutes, shear rate 3000 seconds
-1
, obtain the mixed liquor of emulsion form, then this mixed liquor is input to and carries out second in the high cut disperse emulsification pump and shear, out the part of mixed liquor is fed in the screw extruder from emulsification pump, and remainder loops back solution and twines in the still.In this example, screw extruder is twin-screw, screw extruder diameter 95mm, length-to-diameter is 64,285 ℃ of the temperature of screw rod, rotating speed 160 rpm, the extrudate of screw extruder output pass through behind filter, casing, the measuring pump successively from spinneret orifice (diameter 0.7mm) ejection of spinning pack, then enter in the water-bath that contains the 1wt% surfactant under 20 ℃ and solidify.By the adjustment of the technological parameters such as measuring pump, spinneret draft, obtain the frozen glue precursor of 400D.
(2), to step (1) gained 400D frozen glue precursor leaving standstill under the certain condition, and directly carry out the secondary preliminary draft that multiple is followed successively by 4 times and 2 times, the preliminary draft process is carried out in the air of room temperature.
(3), take agent for carbon hydrogen detergent as extractant, the frozen glue precursor through step (2) is extracted, afterwards, drying obtains total denier 400D, the superhigh molecular weight polyethylene fibers of filament number 2.2D through 31 times hot-stretchs.After testing, fibrous fracture intensity is no more than 33cn/dtex, and modulus is below 1100 g/d, and the denier irregularity of fiber is ± 3%.
Above the present invention has been done detailed description; its purpose is to allow the personage that is familiar with this art can understand content of the present invention and is implemented; can not limit protection scope of the present invention with this; the equivalence that all Spirit Essences according to the present invention are done changes or modifies, and all should be encompassed in protection scope of the present invention
Claims (5)
1. the method for the standby ultrahigh-molecular-weight polyethylene fine denier fibers of a gel spinning legal system, it comprises the frozen glue precursor of (1), preparation ultra-high molecular weight polyethylene; (2), the frozen glue precursor is successively through preliminary draft, extraction, drying and hot-stretch obtain described high molecular weight polyethylene fiber, it is characterized in that: described preliminary draft carries out repeatedly altogether, and repeatedly the general times of preliminary draft is 15～35 times, repeatedly preliminary draft all carries out in 30 ℃～50 ℃ drawing-off medium, described drawing-off medium is air, water or oil, the general times of described hot-stretch is 35～50 times, described method also is included in step (1) afterwards, step (2) is 20 ℃～40 ℃ with described frozen glue precursor in temperature before, humidity is to leave standstill 48～72 hours under 30%～60% the constant temperature and humidity condition.
2. method according to claim 1, it is characterized in that: described drawing-off medium is 30 ℃～40 ℃ air.
3. method according to claim 1, it is characterized in that: described preliminary draft carries out 2～4 times altogether, and drafting multiple reduces one by one, and last pre-draft multiple is 1.1～1.5.
4. method according to claim 3, it is characterized in that: described preliminary draft carries out 3 times altogether.
5. method according to claim 1 is characterized in that: in the step (2), described extraction adopts the alkane of boiling point between 125 ℃～155 ℃ as extractant.
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| CN 201110090624 CN102199798B (en) | 2011-04-12 | 2011-04-12 | Preparation method of ultrahigh-molecular-weight polyethylene fine denier fibers |
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| CN102199798B true CN102199798B (en) | 2013-01-30 |
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| US11230797B2 (en) * | 2011-12-14 | 2022-01-25 | Dsm Ip Assets B.V. | Ultra high molecular weight polyethylene multifilament yarn |
| CN105734708B (en) * | 2014-12-12 | 2018-05-04 | 北京同益中特种纤维技术开发有限公司 | A kind of preparation method of cut resistant superhigh molecular weight polyethylene fibers |
| CN111254511B (en) * | 2020-01-19 | 2022-11-08 | 上海化工研究院有限公司 | Low-temperature spun superfine denier ultra-high molecular weight polyethylene fiber and preparation method thereof |
| CN112941654B (en) * | 2021-01-27 | 2023-10-20 | 上海化工研究院有限公司 | Ultrahigh molecular weight polyethylene fiber and preparation method and application thereof |
Citations (4)
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|---|---|---|---|---|
| CN1995496A (en) * | 2006-12-22 | 2007-07-11 | 中纺投资发展股份有限公司 | Super high molecular weight polyethylene gel method for continuous producing direct spinning fine denier filament |
| CN101591813A (en) * | 2008-05-27 | 2009-12-02 | 宁波荣溢化纤科技有限公司 | A kind of preparation method of super high molecular polyethylene fiber precursor |
| 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 |
| CN101768786A (en) * | 2010-03-10 | 2010-07-07 | 常熟绣珀纤维有限公司 | Preparation method of ultrahigh molecular weight polyethylene fiber |
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| CN101684573B (en) * | 2008-09-27 | 2012-01-04 | 宁波荣溢化纤科技有限公司 | Method for preparing ultra-high molecular weight polyethylene fibers |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1995496A (en) * | 2006-12-22 | 2007-07-11 | 中纺投资发展股份有限公司 | Super high molecular weight polyethylene gel method for continuous producing direct spinning fine denier filament |
| CN101591813A (en) * | 2008-05-27 | 2009-12-02 | 宁波荣溢化纤科技有限公司 | A kind of preparation method of super high molecular polyethylene fiber precursor |
| 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 |
| CN101768786A (en) * | 2010-03-10 | 2010-07-07 | 常熟绣珀纤维有限公司 | Preparation method of ultrahigh molecular weight polyethylene fiber |
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