CN101875779A - Polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material and preparation method thereof - Google Patents
Polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material and preparation method thereof Download PDFInfo
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- CN101875779A CN101875779A CN2009102643527A CN200910264352A CN101875779A CN 101875779 A CN101875779 A CN 101875779A CN 2009102643527 A CN2009102643527 A CN 2009102643527A CN 200910264352 A CN200910264352 A CN 200910264352A CN 101875779 A CN101875779 A CN 101875779A
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Abstract
The invention relates to a polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material and a preparation method thereof. The composite material contains the following components of 100 parts of main substrate polyarylether, 1-6 parts of expanded graphite of which the expansion ratio is more than 100 times, and 1-20 parts of reinforcer carbon fiber. The reinforcer carbon fiber is added to a polyamide/nano expanded graphite compound system to prepare the high-strength high-conductivity composite material. Although the content of the carbon fiber and the expanded graphite is small, the bulk conductivity of the system can reach 10-2S/m, the mechanical properties of the system are excellent, the tensile strength can reach 120.34 MPa, the bending strength reaches 195.51 MPa, and the impact strength is 37.33 KJ/m<2>. The invention has excellent over-all properties, thereby having broad industrialization prospects. The invention is expected to be widely used in the fields of anti-static materials, electromagnetic shielding materials, microwave absorption and the like.
Description
Technical field
The present invention relates to a kind of preparation technology and correlated performance research of polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material, on polyamide/graphite nano conductive composite material preparation method's basis, prepared through the method for simple melt blending intercalation and conducted electricity very well and the polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material of mechanical mechanics property excellence by adding carbon fiber.
Background technology
Polymer base conductive composite material is owing to having that density is little, conductivity is good and chemical resistance is good etc. that advantage obtains promotion and application widely in recent years.But, according to reporting at present with the conducing composite material of polymkeric substance as matrix, how with carbon black, metal powder, metal oxide etc. as conductive filler material, adopt the preparation technology of intercalation polymeric or solution intercalation, this polymer base conductive composite material often needs more conductive filler material just can reach the ideal conductive effect, and conductive filler material content is generally in 15～25% scopes.The increase of filler content and make this type of polymer base conductive composite material processing characteristics and mechanical property variation with interfacial adhesion effect a little less than the matrix, thus limited its application.
Reported in the achievement in research before us and adopted the method for fusion intercalation to prepare polyamide/graphite nano conductive composite material, the polyamide-based graphite nanometer composite material of this method preparation just can obtain higher volume conductance under the less situation of conductive filler material content, its percolation threshold is 3～4%.The content of comparing the inorganic conductive filler with other polymer base conductive composite material has had significantly reduction, thereby has reduced production cost.But the polyamide/graphite nano conductive composite material of this method preparation has so also limited its industrial applications along with the adding of graphite makes the purer polyamide substrate of its mechanical property descend to some extent.
Summary of the invention
The objective of the invention is to invent the good and good processability of a kind of shielding properties, conductivity that had both had better antistatic property, a certain limit, mechanical property excellence, can satisfy the polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material of industrial applications and the preparation method of this matrix material.
The technical scheme that first purpose of the present invention realizes is, the polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material, be made up of at expanded graphite more than 100 times and enhancing body carbon fiber main base polyamide, expansion multiple, the mass parts of each component is: 100 parts of main base polyamide, expansion multiple are at 1～6 part of the expanded graphite more than 100 times, 1～20 part on enhancing body carbon fiber.
Experimental result shows that the present invention has lower percolation threshold and higher specific conductivity and excellent mechanical mechanics property.Carbon fiber is as strongthener, and itself just has excellent conducting performance, therefore along with the adding of carbon fiber, realizes the favorable conductive network in composite inner and expanded graphite, gives the conductivity of main matrix excellence.Simultaneously, carbon fiber also has enhancement, tensile strength, flexural strength and the shock strength etc. of polyamide/nano expanded graphite/carbon fiber matrix material all are greatly improved with respect to pure polyamide substrate, compare also high with other polymer base conductive composite material.Therefore, the polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material has wide industrial prospect, is expected to obtain to use widely in fields such as antistatic material, electromagnetic shielding material, microwave absorbing.
Described main base polyamide is any in nylon 6, nylon 66, nylon 1010, Ni Long11, nylon 12, nylon 46, NYLON610, nylon 612, nylon 1212, the nylon MXD 6.
Described enhancing body carbon fiber is the various trades mark and different length-to-diameter ratio carbon fiber.
Described expanded graphite is a nano expanded graphite, is expansion multiple is placed 24 ± 1 hours in the expanded graphite more than 100 times is dispersed in 70% aqueous ethanolic solution after, obtains nano graphite flakes in ultrasonic 4 ± 0.2 hours.
The technical scheme that second purpose of the present invention realizes is that the preparation method of polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material may further comprise the steps:
1) preparation of nano graphite flakes: natural flake graphite is joined in the mixed solution of the vitriol oil and concentrated nitric acid and soaked 24 ± 3 hours, then with natural flake graphite through washing, after the drying treatment, in being 900～1100 ℃ retort furnace, temperature heats expansion process, obtain expansion multiple at the expanded graphite more than 100 times, again expanded graphite is dispersed in place 24 ± 1 hours in 70% the aqueous ethanolic solution after, obtained nano graphite flakes in ultrasonic 4 ± 0.2 hours;
2) 100 parts of 1～6 part of nano graphite flakes, main base polyamide being mixed the back joins for 1～20 part and can provide shearing force can simultaneously polymkeric substance be heated to again in the equipment more than the fusing point with strengthening the body carbon fiber, melt blending promptly obtains the polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material.
The fineness of described natural flake graphite is 30～200 orders (being that granularity is 100 μ m～500 μ m).
Described main base polyamide is any in nylon 6, nylon 66, nylon 1010, Ni Long11, nylon 12, nylon 46, NYLON610, nylon 612, the nylon 1212.
Described enhancing body carbon fiber is the various trades mark and different length-to-diameter ratio carbon fiber.
The advantage that the present invention utilizes the conductivity of carbon fiber excellence and can be used as the polymkeric substance reinforcing filler, on the basis of obtaining polyamide/graphite nano conductive composite material preparation method achievement in research, by adding carbon fiber, adopt the method for melt blending to prepare the polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material.Concrete grammar is to place high-speed mixer fully to stir the expanded graphite of certain proportioning and main base polyamide, makes it to mix; Then itself and carbon fiber are placed Banbury mixer (as Haake torque rheometer, twin screw extruder etc.) together, be warming up to carry out more than the matrix fusing point mixing, thereby obtain conducing composite material.This preparation method is simple, and cost is lower.
Embodiment
1, preparation expanded graphite:
With granularity is that the natural flake graphite of 100 μ m～500 μ m (fineness is 30～200 orders) joins in the mixed solution that mass ratio is 4: 1 the vitriol oil and concentrated nitric acid and soaked 24 ± 3 hours, then after washing, drying treatment, in being 900～1100 ℃ retort furnace, temperature heats expansion process, obtain expansion multiple at the expanded graphite more than 100 times, standby.
2, preparation nano-graphite:
Expanded graphite is dispersed in 70% the aqueous ethanolic solution and placed 24 ± 1 hours, obtained nano graphite flakes (or claiming nano-graphite or nano expanded graphite) in ultrasonic then 4 ± 0.2 hours, standby.
3, the pre-blend of matrix material
The nano expanded graphite and the main matrix of certain proportioning are placed high-speed mixer, fully stir 10min, the filler nanometer expanded graphite is uniformly dispersed in matrix.
Below main base polyamide be example with nylon 6, specifically illustrate:
Nano expanded graphite accounts for 6 parts of total system mass fraction and 100 parts of main matrix nylon 6 after fully mixing on the high-speed mixer, itself and 2～20 parts are strengthened body carbon fiber material be transferred in the Banbury mixer (Haake torque rheometer or twin screw extruder) mixing 8min under 250 ℃ of conditions respectively, discharging promptly gets the high-strength conductive matrix material.The conductivity data of matrix material and each mechanical performance data see Table one.
Table one
Nano expanded graphite accounts for total system mass fraction 1 part (or 2 parts or 3 parts or 4 parts or 5 parts) and 100 parts of main matrix nylon 6 after fully mixing on the high-speed mixer, itself and 2～20 parts are strengthened body carbon fiber material be transferred in the Banbury mixer (Haake torque rheometer or twin screw extruder) mixing 8min under 250 ℃ of conditions respectively, discharging obtains the high-strength conductive matrix material too.The conductivity data of matrix material and each mechanical performance data are similar to table one.Main base polyamide is 100: 6 with best in quality part ratio of nano expanded graphite.
Main base polyamide makes the high-strength conductive matrix material with nylon 66 or nylon 1010 or Ni Long11 or nylon 12 or nylon 46 or NYLON610 or nylon 612 or nylon 1212 or nylon MXD 6.The conductivity data of matrix material and each mechanical performance data are similar to table one.
Claims (7)
1. polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material, it is characterized in that described matrix material by main base polyamide, expansion multiple at the expanded graphite more than 100 times with strengthen the body carbon fiber and forms, the mass parts of each component is: 100 parts of main base polyamide, expansion multiple are at 1～6 part of the expanded graphite more than 100 times, 1～20 part on enhancing body carbon fiber.
2. according to the described polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material of claim 1, it is characterized in that described main base polyamide is any in nylon 6, nylon 66, nylon 1010, Ni Long11, nylon 12, nylon 46, NYLON610, nylon 612, nylon 1212, the nylon MXD 6.
3. according to the described polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material of claim 1, it is characterized in that described enhancing body carbon fiber is the various trades mark and different length-to-diameter ratio carbon fiber.
4. the preparation method of polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material as claimed in claim 1 is characterized in that may further comprise the steps:
1) preparation of nano graphite flakes: natural flake graphite is joined in the mixed solution of the vitriol oil and concentrated nitric acid and soaked 24 ± 3 hours, then with natural flake graphite through washing, after the drying treatment, in being 900～1100 ℃ retort furnace, temperature heats expansion process, obtain expansion multiple at the expanded graphite more than 100 times, again expanded graphite is dispersed in place 24 ± 1 hours in 70% the aqueous ethanolic solution after, obtained nano graphite flakes in ultrasonic 4 ± 0.2 hours;
2) 100 parts of 1～6 part of nano graphite flakes, main base polyamide are mixed the back and join for 1～20 part and can provide shearing force can simultaneously polymkeric substance be heated to again in the equipment more than the fusing point with strengthening the body carbon fiber, melt blending promptly obtains matrix material.
5. according to the preparation method of the described polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material of claim 4, the fineness that it is characterized in that the natural flake graphite described in the step 1) is 30～200 orders.
6. according to the preparation method of the described polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material of claim 4, it is characterized in that step 2) described in main base polyamide be in nylon 6, nylon 66, nylon 1010, Ni Long11, nylon 12, nylon 46, NYLON610, nylon 612, the nylon 1212 any.
7. according to the preparation method of the described polyamide/nano expanded graphite/carbon fiber high-strength conducting composite material of claim 4, it is characterized in that step 2) described in to strengthen the body carbon fiber be the carbon fiber of different length-to-diameter ratios.
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| CN102604372A (en) * | 2012-02-17 | 2012-07-25 | 南京聚隆科技股份有限公司 | Polyamide composite material with flame retardance and heat conduction and preparation method thereof |
| CN102690514A (en) * | 2011-03-15 | 2012-09-26 | 上海雷博司电器有限公司 | Electromagnetic shielding nylon composite material |
| CN102702730A (en) * | 2012-06-12 | 2012-10-03 | 中国科学院化学研究所 | Fiber/long-carbon-chain nylon in-situ composite material and preparation method |
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- 2009-12-21 CN CN2009102643527A patent/CN101875779A/en active Pending
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| CN102516763A (en) * | 2011-12-12 | 2012-06-27 | 费近峰 | Electromagnetic wave-shielding plastic |
| CN102604372A (en) * | 2012-02-17 | 2012-07-25 | 南京聚隆科技股份有限公司 | Polyamide composite material with flame retardance and heat conduction and preparation method thereof |
| CN102604372B (en) * | 2012-02-17 | 2013-06-05 | 南京聚隆科技股份有限公司 | Polyamide composite material with flame retardance and heat conduction and preparation method thereof |
| CN102702730B (en) * | 2012-06-12 | 2014-07-23 | 中国科学院化学研究所 | Fiber/long-carbon-chain nylon in-situ composite material and preparation method |
| CN102702730A (en) * | 2012-06-12 | 2012-10-03 | 中国科学院化学研究所 | Fiber/long-carbon-chain nylon in-situ composite material and preparation method |
| CN102863787A (en) * | 2012-09-14 | 2013-01-09 | 毛澄宇 | Conductive-antistatic composite material and preparation method thereof |
| CN103740092A (en) * | 2013-12-18 | 2014-04-23 | 江苏悦达新材料科技有限公司 | High-thermal conductivity graphene/nylon composite material and preparation method thereof |
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Open date: 20101103 |