CN103450537B - The preparation method of ultra-high molecular weight polyethylene/graphite alkene anti-static composite material - Google Patents
The preparation method of ultra-high molecular weight polyethylene/graphite alkene anti-static composite material Download PDFInfo
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Abstract
The present invention relates to the preparation method of ultra-high molecular weight polyethylene/graphite alkene anti-static composite material. The method is UHMWPE and graphene powder to be placed in to homogenizer stir, and obtains ultra-high molecular weight polyethylene/graphite alkene composite particles; Graphene powder divides and joins in homogenizer for 2～50 times, stirs 10～30s at every turn, and mixing speed is 10000～30000r/min; By ultra-high molecular weight polyethylene/graphite alkene composite particles preheating 5～10min at 180～240 DEG C, then hot pressing 30min under uniform temp, 10MPa condition, obtains ultra-high molecular weight polyethylene/graphite alkene material. The inventive method does not relate to solvent, prepares by Electrostatic Absorption, then hot-forming, prepares required anti-static composite material. Material prepared by the present invention has three-dimensional net structure, and it is higher that excess effusion value is prepared income value compared with solwution method.
Description
Technical field
The invention belongs to polymeric material field, be specifically related to a kind of ultra-high molecular weight polyethylene/graphite alkene anti-static composite material and preparation method thereof.
Background technology
Ultra-high molecular weight polyethylene is a kind of thermoplastic engineering plastic with Good All-around Property, is bringing into play very important effect in fields such as modernized war and Aeronautics and Astronautics, marine site defend equipment. Ultra-high molecular weight polyethylene has difficult combustion, resist chemical, wear-resisting, electrical insulating property is good and mechanical strength compared with advantages of higher, be widely used in each field, be the general-purpose plastics of output maximum in the world. But ultra-high molecular weight polyethylene sheet resistance is up to 1014Ω～1017Ω easily produces static, easily sets off an explosion and fire, improves the antistatic effect of superhigh molecular weight polyethylene material, can widen its application in fields such as chemical industry, colliery, electronics.
Common compound anti-electrostatic polymer is that the conductive fillers such as carbon black, graphite or metal powder are joined and in single-phase or multiphase polymer, prepare a kind of polymer matrix composite with anti-static function. With the increase of conductive filler, polymer composites, by the transformation occurring from insulator to conductor, exceedes and oozes phenomenon. In order to obtain lower resistivity, conventionally in polymeric matrix, add the filler of high volume integral, as carbon black-filled polymer, need add the filler of 5 ﹪～20 ﹪ volume fractions. Not only cause thus composite processing fluidity variation in process of production, and cause composite materials property decline, production cost to increase.
Graphene, as the two-dimentional conductive filler of one, has high conductivity (6000S/cm), high-specific surface area (2630m2/ g), the excellent properties such as high strength (Young's modulus: 1TPa, ultimate strength: 130GPa). In recent years, some scholars have reported that macromolecule/graphene composite material can realize higher conductance ((S.Stankovich, etal.Nature2006,442:282-286.) under the Graphene content of polar region. Can realize lower excess effusion value (H.Pang, etal.Mater.Lett.2010,64:2226-2229.) and there is special network structure graphene/polymer composite material. The people such as Hu utilize two-step method to prepare isolation structure GNS/UHMWPE composite (H.L.Hu, etal.Carbon2012,50:4596-4599.), first make graphene oxide evenly be coated in UHMWPE particle surface by the method for solution blending, then dried composite particles is added hydrazine hydrate solution situ redox graphene to obtain UHMWPE/ Graphene composite particles, finally obtain UHMWPE/ graphene composite material by the method for hot pressing. The addition that the method is prepared composite Graphene just can be realized exceeding and ooze phenomenon very low in the situation that. But the method is because relate to two step solution blendings, preparation process is comparatively complicated, and need to use hypertoxic chemical reducing agent, as hydrazine hydrate etc., easily causes environmental pollution in industrial mass production process.
Summary of the invention
The object of this invention is to provide a kind of preparation method of ultra-high molecular weight polyethylene/graphite alkene anti-static composite material.
The method is specifically:
Step (1). ultra-high molecular weight polyethylene (UHMWPE) and graphene powder are placed in to homogenizer and stir, obtain ultra-high molecular weight polyethylene/graphite alkene composite particles; The mass ratio of ultra-high molecular weight polyethylene (UHMWPE) and graphene powder is 1000:1～50, and graphene powder divides and joins in homogenizer for 2～50 times, stirs 10～30s at every turn, and mixing speed is 10000～30000r/min;
Step (2). ultra-high molecular weight polyethylene/graphite alkene composite particles prepared by step (1) is by the hot-forming anti-static composite material of preparing, specifically by ultra-high molecular weight polyethylene/graphite alkene composite particles preheating 5～10min at 180～240 DEG C, then hot pressing 30min under uniform temp, 10MPa condition, obtains ultra-high molecular weight polyethylene/graphite alkene material.
The weight average molecular weight of described ultra-high molecular weight polyethylene is 1 × 106～4×106, particle diameter is 80 μ m～200 μ m;
Described Graphene is the graphene powder with single or multiple lift structure, and its diameter is 0.5 μ m～5 μ m, and thickness is 0.5nm～10nm, and specific area is 20m2/g～200m2/ g, electrical conductivity is 800～2000S/cm.
The beneficial effect that the present invention has is:
1. the present invention does not relate to the use of solvent completely in ultra-high molecular weight polyethylene/graphite alkene anti-static composite material process, prepares UHMWPE/ Graphene composite particles by the method for Electrostatic Absorption, then, by hot-forming, prepares required anti-static composite material. The method can not work the mischief to environment, has the possibility of industrial mass production.
2. the ultra-high molecular weight polyethylene/graphite alkene anti-static composite material that prepared by the present invention has three-dimensional net structure, is different from conventional two-dimentional isolation structure material, can obviously observe.
3. it is higher that the excess effusion value of the ultra-high molecular weight polyethylene/graphite alkene anti-static composite material that prepared by the present invention is prepared income value compared with solwution method, but the method departs from the use of the organic solvent such as reducing agent, ethanol completely, realize Green Chemistry, there is industrial mass production prospect completely.
Brief description of the drawings
Fig. 1 is UHMWPE/ graphene composite particle surface sweeping electron microscope picture, wherein (a) is pure UHMWPE particle, (b) for Graphene content be the compound particle of 0.1 ﹪, (c) for Graphene content is the compound particle of 0.5 ﹪, (d) for Graphene content be the compound particle of 1.0 ﹪;
Fig. 2 is the surface sweeping electron microscope picture of UHMWPE/ graphene composite material section, wherein (a) is pure UHMWPE material, (b) for Graphene content be the composite of 0.1 ﹪, (c) for Graphene content is the composite of 0.5 ﹪, (d) for Graphene content be the composite of 1.0 ﹪;
Fig. 3 is that UHMWPE/ graphene composite material electrical conductivity is with Graphene content figure.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further analyzed.
Embodiment 1.
(1) preparation of UHMWPE charged particle: by UHMWPE dry 24h in 100 DEG C of vacuum drying ovens, make in UHMWPE raw material moisture lower than 0.01 ﹪. 10gUHMWPE and 10mg Graphene are placed in to homogenizer and stir, obtain ultra-high molecular weight polyethylene/graphite alkene composite particles; Wherein Graphene divides and joins in homogenizer for 3 times, at every turn with the speed high-speed stirred 10s of 10000r/min.
(2) high temperature is compressing: the ultra-high molecular weight polyethylene/graphite alkene composite particles that step (1) is made is at 200 DEG C of preheating 5min; Then hot pressing 30min under 200 DEG C, 10MPa; Finally under normal pressure, be cooled to normal temperature, prepare target product.
Embodiment 2.
The other the same as in Example 1, the Graphene content adding is 50mg, high-speed stirred number of times is 5 times.
Embodiment 3.
The other the same as in Example 1, the Graphene content adding is 100mg, high-speed stirred number of times is 10 times, adds 10mg Graphene at every turn.
Embodiment 4.
The other the same as in Example 1, the Graphene content adding is 300mg, high-speed stirred number of times is 30 times, adds 10mg Graphene at every turn.
Embodiment 5.
The other the same as in Example 1, the Graphene content adding is 500mg, high-speed stirred number of times is 50 times, adds 10mg Graphene at every turn.
Embodiment 6.
(1) preparation of UHMWPE charged particle: by UHMWPE dry 24h in 100 DEG C of vacuum drying ovens, make in UHMWPE raw material moisture lower than 0.01 ﹪. 10gUHMWPE and 10mg Graphene are placed in to homogenizer and stir, obtain ultra-high molecular weight polyethylene/graphite alkene composite particles; Wherein Graphene divides and joins in homogenizer for 5 times, at every turn with the speed high-speed stirred 10s of 20000r/min.
(3) high temperature is compressing: the ultra-high molecular weight polyethylene/graphite alkene composite particles that step (2) is made is at 200 DEG C of preheating 5min; Then hot pressing 30min under 200 DEG C, 10MPa; Finally be cooled to room temperature under normal pressure again and prepare target product.
Embodiment 7.
Other is with embodiment 6, and the Graphene content adding is 50mg, and high-speed stirred number of times is 5 times, adds 10mg Graphene at every turn.
Embodiment 8.
Other is with embodiment 6, and the Graphene content adding is 100mg, and high-speed stirred number of times is 10 times, adds 10mg Graphene at every turn.
Embodiment 9.
Other is with embodiment 6, and the Graphene content adding is 300mg, and high-speed stirred number of times is 30 times, adds 10mg Graphene at every turn.
Embodiment 10.
Other is with embodiment 6, and the Graphene content adding is 500mg, and high-speed stirred number of times is 50 times, adds 10mg Graphene at every turn.
Embodiment 11.
(1) preparation of UHMWPE charged particle: by UHMWPE dry 24h in 100 DEG C of vacuum drying ovens, make in UHMWPE raw material moisture lower than 0.01 ﹪. 10gUHMWPE and 10mg Graphene are placed in to homogenizer and stir, obtain ultra-high molecular weight polyethylene/graphite alkene composite particles; Wherein Graphene divides and joins in homogenizer for 5 times, at every turn with the speed high-speed stirred 10s of 30000r/min.
(2) high temperature is compressing: the ultra-high molecular weight polyethylene/graphite alkene composite particles that step (1) is made is at 180 DEG C of preheating 10min; Then hot pressing 30min under 200 DEG C, 10MPa; Finally under normal pressure, be cooled to normal temperature, prepare target product.
Embodiment 12.
(1) preparation of UHMWPE charged particle: by UHMWPE dry 24h in 100 DEG C of vacuum drying ovens, make in UHMWPE raw material moisture lower than 0.01 ﹪. 10gUHMWPE and 10mg Graphene are placed in to homogenizer and stir, obtain ultra-high molecular weight polyethylene/graphite alkene composite particles; Wherein Graphene divides and joins in homogenizer for 5 times, at every turn with the speed high-speed stirred 10s of 30000r/min.
(2) high temperature is compressing: the ultra-high molecular weight polyethylene/graphite alkene composite particles that step (1) is made is at 240 DEG C of preheating 8min; Then hot pressing 30min under 200 DEG C, 10MPa; Finally under normal pressure, be cooled to normal temperature, prepare target product.
Feasibility and form and the distribution of graphene conductive network in composite prepared in order to evaluate this conductive polymer composite, the present invention utilizes flying-spot microscope to characterize UHMWPE/ Graphene particle and composite. Find by sem observation, Fig. 1 (a) shows that UHMWPE particle surface exists a large amount of gullies, and this structure makes UHMWPE particle itself have larger specific area, better adsorption of nanoparticles. After mechanical friction, UHMWPE particle surface will, with static, can produce Electrostatic Absorption, add a small amount of Graphene to carry out after high-speed stirred, and Graphene is adsorbed on UHMWPE particle surface by electrostatic interaction, form the UHMWPE particle of graphene coated. Fig. 1 (b) shows that the graphene sheet layer of absorption can be observed in UHMWPE surface when Graphene content is during at 0.1 ﹪, still because Graphene content is lower, can not form complete network structure. Fig. 1 (c) shows in the time that Graphene content reaches 0.5 ﹪, and most of region, UHMWPE surface is covered by Graphene, forms comparatively perfect Graphene network. Fig. 1 (d) shows that while further rising to 1.0 ﹪ along with Graphene content, UHMWPE surface is coated with Graphene completely, can form perfect Graphene network.
The internal structure of the UHMWPE/ graphene composite material by surface sweeping electron microscope observation melting hot pressing, Fig. 2 has shown the section structure of UHMWPE/ graphene composite material. Make discovery from observation, the plane fracture structure that the UHMWPE material showing with respect to Fig. 2 (a) forms, Fig. 2 (b-d) shows that UHMWPE/ graphene composite material has formed the composite structure with three-dimensional net structure. This be because UHMWPE/ graphene composite particle in melting hot pressing, the Graphene of UHMWPE particle surface absorption can form three-dimensional net structure, thereby has stoped the motion of UHMWPE strand. This orderly Graphene network structure can significantly promote the electric conductivity of material.
In order to investigate the electrical conductive behavior of UHMWPE/ Graphene network structural conductive polymer composite prepared by Electrostatic Absorption method, adopt EST121 high resistance measuring instrument and four-point probe measurment instrument to carry out electrical testing to composite, test result is shown in Fig. 3. The Graphene of preparing by our this method has lower excess effusion value (0.1 ﹪) and higher conductance, and addition reaches 1.0 ﹪ can reach anlistatig effect.
In above-described embodiment, the weight average molecular weight of ultra-high molecular weight polyethylene used is 1 × 106～4×106, particle diameter is 80 μ m～200 μ m; Graphene used is the graphene powder with single or multiple lift structure, and its diameter is 0.5 μ m～5 μ m, and thickness is 0.5nm～10nm, and specific area is 20m2/g～200m2/ g, electrical conductivity is 800～2000S/cm.
Above-described embodiment is not that the present invention is not limited only to above-described embodiment for restriction of the present invention, as long as meet requirement of the present invention, all belongs to protection scope of the present invention.
Claims (1)
1. the preparation method of ultra-high molecular weight polyethylene/graphite alkene anti-static composite material, this supra polymerWeight polyethylene/graphite alkene anti-static composite material has three-dimensional net structure, it is characterized in that the method bagDraw together following steps:
Step (1). ultra-high molecular weight polyethylene and graphene powder are placed in to homogenizer and stir,To ultra-high molecular weight polyethylene/graphite alkene composite particles; Ultra-high molecular weight polyethylene and graphene powderMass ratio is 1000:30～50, and graphene powder divides and joins in homogenizer for 2～50 times, eachStir 10～30s, mixing speed is 10000～30000r/min;
Step (2). ultra-high molecular weight polyethylene/graphite alkene composite particles prepared by step (1) is by warmThe molded anti-static composite material of preparing, specifically by ultra-high molecular weight polyethylene/graphite alkene composite particlesPreheating 5～10min at 180～240 DEG C, then hot pressing 30min under uniform temp, 10MPa condition,Obtain ultra-high molecular weight polyethylene/graphite alkene material;
Described Graphene is the graphene powder with single or multiple lift structure, its diameter be 0.5 μ m～5 μ m, thickness is 0.5nm～10nm, specific area is 20m2/g～200m2/ g, electrical conductivity is 800～2000S/cm；
The weight average molecular weight of described ultra-high molecular weight polyethylene is 1 × 106～4×106, particle diameter is 80 μm～200μm。
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| CN104479205B (en) * | 2014-12-09 | 2018-05-04 | 宁波大学 | A kind of injection molding forming method of graphene modified poly ethylene high-strength composite thin products |
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| CN107446221A (en) * | 2017-09-27 | 2017-12-08 | 中玺新材料（安徽）有限公司 | A kind of ultra-high molecular weight polyethylene/graphite alkene composite |
| CN108515172B (en) * | 2018-04-09 | 2021-04-30 | 西安交通大学 | Preparation method of wear-resistant and arc erosion-resistant silver-based material |
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| CN109206712A (en) * | 2018-08-28 | 2019-01-15 | 合肥卓汇新材料科技有限公司 | A kind of processing method of ultra-high molecular weight polyethylene conducing composite material |
| CN109749201A (en) * | 2019-01-03 | 2019-05-14 | 福建师范大学 | A kind of conductive and heat-conductive UHMWPE/ natural flake graphite alkene composite material and preparation method |
| CN116925459B (en) * | 2023-07-20 | 2024-04-16 | 汇仓新材料(苏州)有限公司 | Antistatic PE protective film and preparation method thereof |
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