CN102433600A - Ultrahigh molecular weight polyethylene/carbon black nanometer composite fiber and its preparation method - Google Patents
Ultrahigh molecular weight polyethylene/carbon black nanometer composite fiber and its preparation method Download PDFInfo
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Abstract
The invention provides an ultrahigh molecular weight polyethylene/ carbon black nanometer composite fiber and its preparation method. The method comprises: putting ultrahigh molecular weight polyethylene, carbon black nanoparticles and an anti-oxidant into a solvent, conducting high speed shearing and stirring by an emulsifying machine so as to be uniformly mixed, thus obtaining a mixture; then raising the temperature of the mixture to 100-120DEG C, controlling the temperature raising speed at 2-5DEG C/min, and carrying out thermal insulation for 1-4h so as to obtain a spinning solution, then employing a conventional ultrahigh molecular weight polyethylene fiber production method for preparing an ultrahigh molecular weight polyethylene/carbon black nanometer composite fiber. The ultrahigh molecular weight polyethylene/carbon black nanometer composite fiber prepared in the invention effectively improves the hear resistance and creep resistance of ultrahigh molecular weight polyethylene fibers, reduces fiber production cost, and extends the application scope of fibers. Meanwhile, the preparation method provided in the invention has concise process route and is easy to operate.
Description
Technical field
The present invention relates to a kind of ultra-high molecular weight polyethylene/carbon black nano-composite fiber and preparation method thereof.
Background technology
It is little that ultra-high molecular weight polyethylene has density; UV resistant; Excellent properties such as stable chemical properties such as corrosion-resistant and outstanding shock resistance, anti-cutting toughness; Being one of three big high performance fibre material of generally acknowledging in the world at present, is the ideal material of making soft ballistic protective clothing, anti-stab clothing, lightweight bulletproof helmet, radome, armoured van bulletproof armour, helicopter bulletproof armour, naval vessels and foreign-going ship hawser, lightweight high-pressure bottle, space flight and aviation structural member, deep-sea wind wave-resisting net casing, fishing net, racing boat, sailing boat, sled etc.Yet, because the molecular weight of ultra-high molecular weight polyethylene is bigger, up to more than 1,000,000; Strand is very long, very easily tangles, and is mobile relatively poor, is difficult to processing.And because the macromolecular structure of ultra-high molecular weight polyethylene is a linear structure; Form by the methylene group; No any polar group on the strand; So its heat resistance poor (serviceability temperature generally is lower than 100 ℃), creep is serious, thereby has limited the range of application of superhigh molecular weight polyethylene fibers.The heat resistance and the creep resistance that how to change superhigh molecular weight polyethylene fibers have become the important topic that further develops superhigh molecular weight polyethylene fibers.
At present, improve the heat resistance of superhigh molecular weight polyethylene fibers and the method for creep resistance and mainly contain following several kinds:
The one, make the fiber self-crosslinking.Make the superhigh molecular weight polyethylene fibers self-crosslinking can be divided into chemical crosslinking and crosslinking with radiation.So-called chemical crosslinking is exactly after ultra-high molecular weight polyethylene adds the proper crosslinking agent, in melting process, takes place crosslinked; Because the molecular weight of ultra-high molecular weight polyethylene is very big, is difficult for fusion, and nonpolarity group on the strand; So chemical crosslinking is difficult for carrying out; The effect of modification is not clearly, and in cross-linking process, also degradation reaction can take place, and the performance of ultra-high molecular weight polyethylene is reduced.So-called crosslinking with radiation; Be utilize high-energy radiation to make between strand to produce laterally crosslinked; It can improve the heat resistance and the creep-resistant property of superhigh molecular weight polyethylene fibers to a certain extent, but in crosslinked process, also inevitably produces chain-scission degradation, along with the increase of dosage of radiation; Palliating degradation degree also increases, and the TENSILE STRENGTH of fiber and extension at break are decreased; In addition, this technical process is comparatively complicated.
The 2nd, add medium molecular weight polyvinyl.The polyethylene that in ultra-high molecular weight polyethylene, adds intermediate molecular weight comprises adding low density polyethylene (LDPE) (LDPE) and high density polyethylene (HDPE) (HDPE).Though the affiliation that adds of LDPE and HDPE makes moderate progress the flowability of UHMWPE, make the mechanical property of UHMWPE reduce a lot.
The 3rd, add inorganic filler.Add suitable inorganic filler at ultra-high molecular weight polyethylene; As add silica, alchlor, mica, talcum powder, imvite etc.; The filler that adds plays the effect of crystallization nucleating agent or physical crosslinking point, has limited the warm-up movement of molecule, can improve the heat resistance and the creep resistance of fiber; But filler also becomes stress concentration point simultaneously, causes the impact strength of fiber to descend.
The 4th, use with other high-performance fiber.Superhigh molecular weight polyethylene fibers and Tan Xian Wei ﹑ glass fibre and Kevlar is fiber blended; Also can improve its heat resistance and creep resistance; But owing to do not have polar group and smooth surface on the ultra-high molecular weight polyethylene strand, can not and use with and form compatible interface between fiber, can not form good active force between two components; And add the mobile variation that these fibers also can make ultra-high molecular weight polyethylene, be difficult to processing.
Chinese patent 03115230.9 discloses a kind of gel-spun ultra-high molecular weight polyethylene/carbon nano tube composite fibre and preparation thereof; It is in spinning solution, to add through purifying and the CNT that organises and handle; Make gel-spun ultra-high molecular weight polyethylene/carbon nano tube composite fibre, make the heat resistance of composite fibre and creep resistance improve.But because the CNT expensive makes that the composite fibre cost of preparation is higher, and CNT will pass through purifying and the processing that organises, and operation is numerous and diverse, has caused certain difficulty to suitability for industrialized production.
Summary of the invention
For overcoming the weak point of prior art, the present invention provides a kind of super high molecular weight ultra-high molecular weight polyethylene/carbon black nano-composite fiber, to improve the heat resistance and the creep resistance of ultrahigh molecular weight (UHMW) polyethylene fiber, enlarges its scope of application; The present invention simultaneously also provides the preparation method of a kind of above-mentioned super high molecular weight ultra-high molecular weight polyethylene/carbon black nano-composite fiber, and its process route is succinct, easy operating.
The technical solution adopted for the present invention to solve the technical problems is:
Ultra-high molecular weight polyethylene of the present invention/carbon black nano-composite fiber is made up of ultra-high molecular weight polyethylene and carbon black nano particle; The content of nano carbon particle is 0.1～5% of total weight of fiber.
The preparation method of above-mentioned ultra-high molecular weight polyethylene/carbon black nano-composite fiber comprises the steps:
(1) with in ultra-high molecular weight ultra-high molecular weight polyethylene, carbon black nano particle and anti-oxidant and the input solvent, stir through the mulser high speed shear, mix, obtain compound;
(2) above-mentioned gained compound is warming up to 100～120 ℃, programming rate is controlled at 2～5 ℃/min, is incubated 1～4 hour, obtains spinning solution;
(3) spinning solution adopts conventional process for preparing ultrahigh molecular weight polyethylene fibre, makes ultra-high molecular weight polyethylene/carbon black nano-composite fiber.
In the above-mentioned steps (1), the parts by weight of super high molecular weight ultra-high molecular weight polyethylene, carbon black nano particle and anti-oxidant are: 95～99.8,0.1～5 and 0.1～1 part.
The Fen Ziliang > of said ultra-high molecular weight polyethylene; 2 * 10
6G/mol.
The diameter of said carbon black nano particle is 100～1000nm.
Described solvent is one or several in white oil, paraffin oil, decahydronaphthalenes, the mineral oil; The viscosity of solvent is 40～100Cst under 40 ℃.
Described anti-oxidant is 2,6-di-tert-butyl methyl phenol or N-phenyl--naphthylamines.
The speed of above-mentioned steps (1) high speed shear agitation is 1000～3000r/min, and mixing time is 0.5～1h.
The concentration of spinning solution is 5%～20% described in the above-mentioned steps (2).
Beneficial effect of the present invention is: prepared ultra-high molecular weight polyethylene/carbon black nano-composite fiber; Owing to added carbon black nano particle with excellent properties; In the process that superhigh molecular weight polyethylene fibers is stretched, form certain orientation; Reveal more performance than other modifier (like inorganic filler and fiber etc.) and ultra-high molecular weight polyethylene composite table, thereby improve the heat resistance and the creep resistance of superhigh molecular weight polyethylene fibers, enlarged the scope of application of fiber; And, greatly reduce the production cost of this fiber because the carbon black nano particle is cheap than CNT.Simultaneously, preparation method provided by the present invention, its process route is succinct, easy operating.
The specific embodiment
Below in conjunction with embodiment the present invention is further specified.
Embodiment 1:
With parts by weight is that (granularity 80 orders, mean molecule quantity are 4.5 * 10 for 99.4 parts ultra-high molecular weight polyethylene powder
6G/mol), 0.5 part carbon black nano particle (its particle diameter is 100nm) and 0.1 part are as 2 of antioxidant; The 6-di-tert-butyl methyl phenol; Drop in 900 parts of white oils (its viscosity is 50Cst down at 40 ℃) solvent; In mulser, stir 1h, obtain uniform compound with 1000 rev/mins of high speed shear; Compound is incubated 1 hour after being warming up to 110 ℃ with the programming rate of 2 ℃/min, and obtaining concentration is 10% uniform spinning solution; Spinning solution is fed double screw extruder.The double screw extruder diameter is 95mm, L/D=(68), and temperature is controlled at 240 ℃, rotating speed 120 commentaries on classics/min.From the shower nozzle ejection, through extraction after the water bath processing, dry and hot drawing-off, draw ratio is 60 times to extrudate, obtains ultra-high molecular weight polyethylene/carbon black nano-composite fiber after filtering, measuring.
Embodiment 2:
With parts by weight is that (granularity 90 orders, mean molecule quantity are 4 * 10 for 98.7 parts ultra-high molecular weight polyethylene powder
6G/mol), 1 part carbon black nano particle (its particle diameter is 300nm) and 0.3 part of N-phenyl as antioxidant--naphthylamines; Drop in 900 parts the decahydronaphthalenes as solvent (its viscosity is down 70Cst at 40 ℃); In mulser, stir 1h, the compound that obtains mixing with 2000 rev/mins of high speed shear; Compound is incubated 4 hours after being warming up to 100 ℃ with the programming rate of 3 ℃/min, and obtaining concentration is 10% spinning solution.Adopt the method identical, spinning solution is made ultra-high molecular weight polyethylene/carbon black nano-composite fiber with embodiment 1.
Embodiment 3:
With parts by weight is that (granularity 100 orders, mean molecule quantity are 3 * 10 for 96 parts ultra-high molecular weight polyethylene powder
6G/mol), 3 parts carbon black nano particle (its particle diameter is 500nm) and 1 part of N-phenyl as antioxidant--naphthylamines; Drop in 400 parts the paraffin oil as solvent (its viscosity is down 80Cst at 40 ℃); In mulser, stir 0.5h, the compound that obtains mixing with 3000 rev/mins of high speed shear; Compound is incubated 2 hours after being warming up to 120 ℃ with the programming rate of 5 ℃/min, and obtaining concentration is 20% spinning solution.Adopt the method identical, spinning solution is made ultra-high molecular weight polyethylene/carbon black nano-composite fiber with embodiment 1.
Embodiment 4:
With parts by weight is that (granularity 120 orders, mean molecule quantity are 5 * 10 for 95 parts ultra-high molecular weight polyethylene powder
6G/mol), 4.8 parts carbon black nano particle (its particle diameter is 1000nm), 0.2 part of N-phenyl as antioxidant--naphthylamines; Drop in 1900 parts the paraffin oil as solvent (its viscosity is down 80Cst at 40 ℃); In mulser, stir 0.5h, the compound that obtains mixing with 3000 rev/mins of high speed shear; Compound is incubated 1 hour after being warming up to 120 ℃ with the programming rate of 4 ℃/min, and obtaining concentration is 5% spinning solution.Adopt the method identical, spinning solution is made ultra-high molecular weight polyethylene/carbon black nano-composite fiber with embodiment 1.
Comparative example 1:
(granularity 80 orders, molecular weight are 4.5 * 10 to the ultra-high molecular weight polyethylene powder
6G/mol), dissolvant white oil and antioxidant 2,6-di-tert-butyl methyl phenol; To be made into concentration be 10% suspension to 89.9:10:0.1 by mass percentage, under the nitrogen protection effect, is warming up to 110 ℃ with the speed of 2 ℃/min; Speed with 60 commentaries on classics/min stirs simultaneously; Be incubated 1 hour, obtain uniform spinning solution, then through side drawing-in device feeding double screw extruder.The double screw extruder diameter is 95mm, L/D=(68), and temperature is controlled at 240 ℃, rotating speed 160 commentaries on classics/min.From the shower nozzle ejection, through extraction after the water bath processing, dry and hot drawing-off, draw ratio is 60 times to extrudate, obtains superhigh molecular weight polyethylene fibers after filtering, measuring.
Comparative example 2:
Adopt the embodiment 1 said method and the result thereof of Chinese patent 03115230.9 record.
The performance comparison sheet of table 1: embodiment and the said fiber of comparative example
Find relatively that through table 1 the more existing superhigh molecular weight polyethylene fibers of modulus, intensity, creep resistance and heat resistance (comparative example 1) of the ultra-high molecular weight polyethylene that the present invention makes/carbon black nano-composite fiber (embodiment 1-4) is significantly improved; With existing ultra-high molecular weight polyethylene/carbon nano tube composite fibre (comparative example 2), intensity, modulus, creep resistance and heat resistance are suitable.
Claims (9)
1. ultra-high molecular weight polyethylene/carbon black nano-composite fiber is characterized in that: be made up of ultra-high molecular weight polyethylene and carbon black nano particle; The content of carbon black nano particle is 0.1～5% of total weight of fiber.
2. a preparation method who realizes the described ultra-high molecular weight polyethylene of claim 1/carbon black nano particle composite fibre is characterized in that: comprise the steps:
(1) with in ultra-high molecular weight ultra-high molecular weight polyethylene, carbon black nano particle and anti-oxidant and the input solvent, stir through the mulser high speed shear, mix, obtain compound;
(2) above-mentioned gained compound is warming up to 100～120 ℃, programming rate is controlled at 2～5 ℃/min, is incubated 1～4 hour, obtains spinning solution;
(3) spinning solution adopts conventional process for preparing ultrahigh molecular weight polyethylene fibre, makes ultra-high molecular weight polyethylene/carbon black nano-composite fiber.
3. the preparation method of 2 described a kind of ultra-high molecular weight polyethylene/carbon black nano-composite fibers as requested; It is characterized in that: in the above-mentioned steps (1), the parts by weight of super high molecular weight ultra-high molecular weight polyethylene, carbon black nano particle and anti-oxidant are: 95～99.8,0.1～5 and 0.1～1 part.
4. the preparation method of 2 described a kind of ultra-high molecular weight polyethylene/carbon black nano-composite fibers as requested is characterized in that: the Fen Ziliang > of said ultra-high molecular weight polyethylene; 2 * 10
6G/mol.
5. the preparation method of 2 described a kind of ultra-high molecular weight polyethylene/carbon black nano-composite fibers as requested, it is characterized in that: the diameter of said carbon black nano particle is 100～1000nm.
6. the preparation method of 2 described a kind of ultra-high molecular weight polyethylene/carbon black nano-composite fibers as requested, it is characterized in that: described solvent is one or several in white oil, paraffin oil, decahydronaphthalenes, the mineral oil; The viscosity of solvent is 40～100Cst under 40 ℃.
7. the preparation method of 2 described a kind of ultra-high molecular weight polyethylene/carbon black nano-composite fibers as requested, it is characterized in that: described anti-oxidant is 2,6-di-tert-butyl methyl phenol or N-phenyl--naphthylamines.
8. the preparation method of 2 described a kind of ultra-high molecular weight polyethylene/carbon black nano-composite fibers as requested, it is characterized in that: the speed of above-mentioned steps (1) high speed shear agitation is 1000～3000r/min, and mixing time is 0.5～1h.
9. the preparation method of 2 described a kind of ultra-high molecular weight polyethylene/carbon black nano-composite fibers as requested, it is characterized in that: the concentration of spinning solution is 5%～20% described in the above-mentioned steps (2).
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| CN104233497A (en) * | 2014-09-17 | 2014-12-24 | 江苏锵尼玛新材料有限公司 | Preparation method and application of UHMWPE (ultra-high molecular weight polyethylene) fiber with high cut resistance |
| CN106192199A (en) * | 2016-08-09 | 2016-12-07 | 中国水产科学研究院东海水产研究所 | A kind of sea fishery is with knotting |
| CN106192030A (en) * | 2016-08-09 | 2016-12-07 | 淄博美标高分子纤维有限公司 | Far-reaching sea net cage or drift line type purse seine are with antifouling melt-spun slivers processing method |
| CN106192065A (en) * | 2016-08-09 | 2016-12-07 | 中国水产科学研究院东海水产研究所 | Krill fishery or the Culture pure seine manufacture method of superpower antibacterial melt-spun silk |
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| EP3107961A4 (en) * | 2014-02-20 | 2017-11-01 | Reliance Industries Limited | High strength and high modulus ultra-high molecular weight polyethylene fibers |
| CN107313124A (en) * | 2017-06-23 | 2017-11-03 | 安徽长青藤新材料有限公司 | Ultrashort fine enhancing ultra-high molecular weight polyethylene composite fibre and its manufacture method |
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| CN113026135A (en) * | 2021-03-15 | 2021-06-25 | 浙江千禧龙纤特种纤维股份有限公司 | Ultra-high molecular weight polyethylene fiber anti-cutting bag, anti-cutting bag material and preparation method thereof |
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| CN115233329A (en) * | 2016-09-27 | 2022-10-25 | 帝斯曼知识产权资产管理有限公司 | UHMWPE fibers, yarns and articles thereof |
| CN107313124A (en) * | 2017-06-23 | 2017-11-03 | 安徽长青藤新材料有限公司 | Ultrashort fine enhancing ultra-high molecular weight polyethylene composite fibre and its manufacture method |
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Application publication date: 20120502 |