CN102924910B - Method of preparing high-performance glass-fiber reinforced polyamide conductive composite - Google Patents
Method of preparing high-performance glass-fiber reinforced polyamide conductive composite Download PDFInfo
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Abstract
The invention relates to a method of preparing a high-performance glass-fiber reinforced polyamide conductive composite. The method comprises the following steps that by the role of electrostatic force between opposite charges, a carbon nano tube and an ethylene/maleic anhydride copolymer are coated on the surface of glass fiber to form a multi-fiber mixed reinforcement structure; and the carbon nano tube/nylon masterbatch and nylon resin are uniformly mixed and then are compounded with the glass fiber reinforcement through an extrusion molding process, so as to obtain a high-performance glass-fiber reinforced nylon conductive composite. The reaction steps of the method are simple, the obtained composite has a good mechanical property and a good conductivity property and can be applied to the fields of automobile industry, electron and electricity, machinery and the like, and the range of application of the glass-fiber reinforced nylon composite is widened.
Description
Technical field
The present invention relates to a kind of nylon composite materials, particularly a kind of preparation method of high-performance glass fiber reinforced polyamide conducing composite material.
Background technology
Nylon is as output maximum in the world, engineering plastics that range of application is the widest, and it is high that it has mechanical strength; Good self lubricity and wear resistance; Wearability, chemical proofing; Processing characteristics excellence, is easy to the advantages such as machine-shaping.Be widely used in automotive industry, the field such as electric, mechanical.
Along with the industries such as automobile, electronic apparatus, communication, machinery are more and more stronger to the high performance requirement of product, need to nylon, carry out modification by certain method, it is developed to high performance engineering plastics and functional plastics by direct labor engineering plastics.The method of modifying of nylon mainly contains: (1) fiber reinforcement; (2) elastic body toughening; (3) high polymer alloy; (4) nanometer particle-modified.Wherein fiber reinforced nylon is the Main Means of nylon enhancing modified, and glass fibre is the main reinforcing filler of nylon.Interface combination between fluoropolymer resin and glass fibre is a very important important factor that affects composite property.Due to the interface between glass fibre and resin matrix, be combined poorly, conventionally need to carry out surface modification to glass fibre.The glass fibre that adds high-content in polymeric matrix can cause fluidity of molten poor simultaneously, is difficult to the problems such as machine-shaping, causes the mechanical property of glass fibre reinforced nylon matrix material to be difficult to further lifting.Thereby simple glass fibre reinforced nylon system can only single and limitedly strengthen mechanical property, cannot make better lifting at aspects such as improving system electroconductibility and thermotolerance, limited further developing and applying of nylon.
Carbon nanotube has superpower mechanical property, greatly length-to-diameter ratio, good electric property, very high chemistry and thermostability etc., and these good character make carbon nanotube be considered to the strongthener of desirable polymer composites just.But the real potential of carbon nanotube does not obtain due embodiment in the material of macro-scale, the increase rates such as the intensity modulus to material are limited, far below traditional strongthener, this is mainly because carbon nanotube exists difficult dispersion and interface in conjunction with poor problem, thereby is restricted in the application of the high-end field of structural part and alternative metals material.Generally speaking, the effect of independent carbon nano-tube modification polymkeric substance is undesirable, and carbon nanotube is restricted as the application of a kind of enhancing and conductive filler material.
Summary of the invention
The object of the invention is to provide a specific admixture glass fibre reinforcement, with and with the compound preparation method who obtains high-performance conductive matrix material of nylon/carbon nanotube system.
The present invention proposes a kind of preparation method of high-performance glass fiber reinforced nylon conducing composite material, utilize glass fibre and the carbon nanotube of surface band negative charge and the electrostatic adsorption of ethene/copolymer-maleic anhydride of surface band positive charge, at fiberglass surfacing enveloped carbon nanometer tube and ethene/copolymer-maleic anhydride, obtain the glass fibre reinforcement of multi-dimensional hybrid; Nylon is mixed with carbon nano-tube/nylon master batch, after method with this glass fibre reinforcement by extrusion moulding is compound, obtain high performance glass fibre reinforced nylon conducing composite material.Concrete steps are as follows:
A preparation method for high-performance glass fiber reinforced polyamide conducing composite material, comprises the steps:
(1) take 1～20g ethene/copolymer-maleic anhydride, mix with the deionized water of 3～5L, in 10r/min～10
3r/min centrifugal speed stirs the lower 1～12h of processing, obtains the aqueous solution of ethene/copolymer-maleic anhydride;
(2) take the carbon nanotube that 2～20g is dry, add in the aqueous solution of described ethene/copolymer-maleic anhydride, in ultrasonic wave and 10r/min～10 of 60～120kHz
3r/min centrifugal speed stirs the lower 1～12h of processing, obtains the suspension that carbon nanotube and ethene/copolymer-maleic anhydride coexist;
(3) taking 10～1000g commercialization glass fibre adds in described suspension, in 10r/min～10
3under r/min centrifugal speed, stir the lower 1～60min of processing, outwell supernatant liquid, repeatedly by washed with de-ionized water to remove the particle not being coated on glass fibre, obtain the multi-dimensional hybrid glass fibre reinforcement of fiberglass surfacing enveloped carbon nanometer tube and ethene/copolymer-maleic anhydride after dry;
(4) nylon resin is mixed with carbon nano-tube/nylon master batch, then by extruding-out process, undertaken compound with described multi-dimensional hybrid glass fibre reinforcement; By following weight ratio, take material:
Nylon resin: 60～80 weight parts;
Multi-dimensional hybrid glass fibre reinforcement: 15～35 weight parts;
Carbon nano-tube/nylon master batch: 5～8 weight parts;
Oxidation inhibitor: 0.15～0.25 weight part;
(5) material after compound step (4) is extruded and granulation through twin screw extruder, wherein said multi-dimensional hybrid glass fibre reinforcement is added by side feeding, the screw speed of described twin screw extruder is 120～600 revs/min, temperature is 265～280 ℃, obtains described high-performance glass fiber reinforced polyamide conducing composite material.
Described ethene/copolymer-maleic anhydride is poly-(ethene-alt-maleic anhydride).
Described carbon nanotube is multi-walled carbon nano-tubes, and mean diameter is 10～20nm, and mean length is 3 μ m left and right, purity > 90 % by weight.
Described commercialization glass fibre is aminosilane coated glass fiber.
Described nylon resin is nylon 6 or nylon 66, and wherein the fusing point of nylon is 225 ℃, and the fusing point of nylon 66 is 265 ℃.
The formation of described carbon nano-tube/nylon master batch is: carbon nanotube: 15%, nylon master batch 66:85%; The fusing point of described carbon nano-tube/nylon master batch is 263 ℃; Described carbon nanotube is multi-walled carbon nano-tubes, and described nylon master batch is nylon 66.
Described oxidation inhibitor is the compound system of Hinered phenols antioxidant and phosphite ester kind antioxidant.
What in the present invention, adopt that the method for electrostatic adhesion prepares mixes glass fibre reinforcement, and its preparation method is simple, without special processing.The carbon nanotube of fiberglass surfacing can be given the certain conductivity of glass fibre of electrical isolation, thereby improves the specific conductivity of matrix material; The anhydride group of the ethene/copolymer-maleic anhydride of fiberglass surfacing can with nylon matrix generation chemical reaction, make nylon form crosslinking structure to a certain degree, and can further improve the interface binding intensity between fiber and nylon resin, the mechanical property of above-mentioned glass fiber enhanced nylon matrix material is effectively improved, due to its excellent mechanical property and conductivity, can be applied to automotive industry, the field such as electric, mechanical, widen glass fibre reinforced nylon prepare composite.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the glass-fibre reinforced polyamide conducing composite material of embodiment 1.
Embodiment
Further illustrate content of the present invention with embodiment, but protection scope of the present invention is not limited in embodiment below.The other changes and modifications that those skilled in the art is made in the situation that not deviating from the present invention's spirit and protection domain, within being still included in protection domain of the present invention.
Embodiment 1
Preparation carbon nanotube concentration is the suspension that 2g/L, ethene/copolymer-maleic anhydride concentration are 1g/L, after supersound process, add the glass fibre of concentration 200g/L, utilize the electrostatic adsorption between the positive charge of fiberglass surfacing and the negative charge on carbon nanotube and ethene/copolymer-maleic anhydride surface, obtain the glass fibre reinforcement that multi-dimensional hybrid strengthens; Carbon nano-tube/nylon master batch is mixed with nylon resin, compound by the technique of extrusion moulding with above-mentioned glass fibre reinforcement again, obtain high-performance glass fiber reinforced nylon conducing composite material, in this matrix material, contain 30% glass fibre reinforcement and 6.7% carbon nano-tube/nylon master batch.
Step (1): in the beaker of 5L, add 3g ethene/copolymer-maleic anhydride and 3L deionized water, stir process 12h, obtains the aqueous solution of ethene/copolymer-maleic anhydride;
Step (2): take the carbon nanotube that 6g is dry, join in the aqueous solution of step (1) gained, process and stir 1h under the ultrasonic wave of 120kHz, obtain the suspension that carbon nanotube and ethene/copolymer-maleic anhydride coexist;
Step (3): take in the suspension that 600g commercialization glass fibre adds gained in step (2) to, stir process 20min, outwell supernatant liquid, repeatedly by washed with de-ionized water to remove the particle not being coated on glass fibre, 80 ℃ of dry 12h, obtain being coated with the multi-dimensional hybrid glass fibre reinforcement of carbon nanotube and ethene/copolymer-maleic anhydride;
Step (4): nylon resin is mixed with carbon nano-tube/nylon master batch, then with step (3) in the glass fibre reinforcement that mixes of gained by extruding-out process, undertaken compoundly, by following weight ratio, take material:
Nylon resin: 63.1 weight parts;
Multi-dimensional hybrid glass fibre reinforcement: 30 weight parts;
Carbon nano-tube/nylon master batch: 6.7 weight parts;
Oxidation inhibitor: 0.15～0.25 weight part;
Step (5): above-mentioned material is extruded and granulation through twin screw extruder, wherein glass fibre reinforcement is added by side feeding, extruder screw rotating speed is 120 revs/min, and temperature is 265 ℃, can obtain high-performance glass fiber reinforced polyamide conducing composite material.
Fig. 1 is the scanning electron microscope (SEM) photograph of the glass-fibre reinforced polyamide conducing composite material prepared while being 1g/L of ethene/copolymer-maleic anhydride strength of solution.
Embodiment 2
Preparation carbon nanotube concentration is the suspension that 2g/L, ethene/copolymer-maleic anhydride concentration are 1.5g/L, after supersound process, add the glass fibre of concentration 200g/L, utilize the electrostatic adsorption between the positive charge of fiberglass surfacing and the negative charge on carbon nanotube and ethene/copolymer-maleic anhydride surface, obtain the glass fibre reinforcement that multi-dimensional hybrid strengthens; Carbon nano-tube/nylon master batch is mixed with nylon resin, more compound by the technique of extrusion moulding with above-mentioned glass fibre reinforcement, obtain high-performance glass fiber reinforced nylon conducing composite material.In this matrix material, contain 30% glass fibre reinforcement and 6.7% carbon nano-tube/nylon master batch.
Step (1): in the beaker of 5L, add 4.5g ethene/copolymer-maleic anhydride and 3L deionized water, stir process 12h, obtains the aqueous solution of ethene/copolymer-maleic anhydride;
Step (2): take the carbon nanotube that 6g is dry, join in the aqueous solution of step (1) gained, process and stir 1h under the ultrasonic wave of 120kHz, obtain the suspension that carbon nanotube and ethene/copolymer-maleic anhydride coexist;
Step (3): take in the suspension that 600g commercialization glass fibre adds gained in step (2) to, stir process 20min, outwell supernatant liquid, repeatedly by washed with de-ionized water to remove the particle not being coated on glass fibre, 80 ℃ of dry 12h, obtain being coated with the multi-dimensional hybrid glass fibre reinforcement of carbon nanotube and ethene/copolymer-maleic anhydride;
Step (4): nylon resin is mixed with carbon nano-tube/nylon master batch, then with step (3) in the glass fibre reinforcement that mixes of gained by extruding-out process, undertaken compoundly, by following weight ratio, take material:
Nylon resin: 63.1 weight parts;
Multi-dimensional hybrid glass fibre reinforcement: 30 weight parts;
Carbon nano-tube/nylon master batch: 6.7 weight parts;
Oxidation inhibitor: 0.15～0.25 weight part;
Step (5): above-mentioned material is extruded and granulation through twin screw extruder, wherein glass fibre reinforcement is added by side feeding, extruder screw rotating speed is 120 revs/min, and temperature is 265 ℃, can obtain high-performance glass fiber reinforced polyamide conducing composite material.
Embodiment 3
Preparation carbon nanotube concentration is the suspension that 2g/L, ethene/copolymer-maleic anhydride concentration are 2g/L, after supersound process, add the glass fibre of concentration 200g/L, utilize the electrostatic adsorption between the positive charge of fiberglass surfacing and the negative charge on carbon nanotube and ethene/copolymer-maleic anhydride surface, obtain the glass fibre reinforcement that multi-dimensional hybrid strengthens; Carbon nano-tube/nylon master batch is mixed with nylon resin, compound by the technique of extrusion moulding with above-mentioned glass fibre reinforcement again, obtain high-performance glass fiber reinforced nylon conducing composite material, in this matrix material, contain 30% glass fibre reinforcement and 6.7% carbon nano-tube/nylon master batch.
Step (1): in the beaker of 5L, add 6g ethene/copolymer-maleic anhydride and 3L deionized water, stir process 12h, obtains the aqueous solution of ethene/copolymer-maleic anhydride;
Step (2): take the carbon nanotube that 6g is dry, join in the aqueous solution of step (1) gained, process and stir 1h under the ultrasonic wave of 120kHz, obtain the suspension that carbon nanotube and ethene/copolymer-maleic anhydride coexist;
Step (3): take in the suspension that 600g commercialization glass fibre adds gained in step (2) to, stir process 20min, outwell supernatant liquid, repeatedly by washed with de-ionized water to remove the particle not being coated on glass fibre, 80 ℃ of dry 12h, obtain being coated with the multi-dimensional hybrid glass fibre reinforcement of carbon nanotube and ethene/copolymer-maleic anhydride;
Step (4): nylon resin is mixed with carbon nano-tube/nylon master batch, then with step (3) in the glass fibre reinforcement that mixes of gained by extruding-out process, undertaken compoundly, by following weight ratio, take material:
Nylon resin: 63.1 weight parts;
Multi-dimensional hybrid glass fibre reinforcement: 30 weight parts;
Carbon nano-tube/nylon master batch: 6.7 weight parts;
Oxidation inhibitor: 0.15～0.25 weight part;
Step (5): above-mentioned material is extruded and granulation through twin screw extruder, wherein glass fibre reinforcement is added by side feeding, extruder screw rotating speed is 120 revs/min, and temperature is 265 ℃, can obtain high-performance glass fiber reinforced polyamide conducing composite material.
Embodiment 4
Preparation carbon nanotube concentration is the suspension that 2g/L, ethene/copolymer-maleic anhydride concentration are 1g/L, after supersound process, add the glass fibre of concentration 200g/L, utilize the electrostatic adsorption between the positive charge of fiberglass surfacing and the negative charge on carbon nanotube and ethene/copolymer-maleic anhydride surface, obtain the glass fibre reinforcement that multi-dimensional hybrid strengthens; Carbon nano-tube/nylon master batch is mixed with nylon resin, compound by the technique of extrusion moulding with above-mentioned glass fibre reinforcement again, obtain high-performance glass fiber reinforced nylon conducing composite material, in this matrix material, contain 25% glass fibre reinforcement and 6.7% carbon nano-tube/nylon master batch.
Step (1): in the beaker of 5L, add 6g ethene/copolymer-maleic anhydride and 3L deionized water, stir process 12h, obtains the aqueous solution of ethene/copolymer-maleic anhydride;
Step (2): take the carbon nanotube that 6g is dry, join in the aqueous solution of step (1) gained, process and stir 1h under the ultrasonic wave of 120kHz, obtain the suspension that carbon nanotube and ethene/copolymer-maleic anhydride coexist;
Step (3): take in the suspension that 600g commercialization glass fibre adds gained in step (2) to, stir process 20min, outwell supernatant liquid, repeatedly by washed with de-ionized water to remove the particle not being coated on glass fibre, 80 ℃ of dry 12h, obtain being coated with the multi-dimensional hybrid glass fibre reinforcement of carbon nanotube and ethene/copolymer-maleic anhydride;
Step (4): nylon resin is mixed with carbon nano-tube/nylon master batch, then with step (3) in the multi-dimensional hybrid glass fibre reinforcement of gained by extruding-out process, undertaken compoundly, by following weight ratio, take material:
Nylon resin: 68.1 weight parts;
Multi-dimensional hybrid glass fibre reinforcement: 25 weight parts;
Carbon nano-tube/nylon master batch: 6.7 weight parts;
Oxidation inhibitor: 0.15～0.25 weight part;
Step (5): above-mentioned material is extruded and granulation through twin screw extruder, wherein glass fibre reinforcement is added by side feeding, extruder screw rotating speed is 120 revs/min, and temperature is 265 ℃, can obtain high-performance glass fiber reinforced polyamide conducing composite material.
Embodiment 5
Preparation carbon nanotube concentration is the suspension that 2g/L, ethene/copolymer-maleic anhydride concentration are 1g/L, after supersound process, add the glass fibre of concentration 200g/L, utilize the electrostatic adsorption between the positive charge of fiberglass surfacing and the negative charge on carbon nanotube and ethene/copolymer-maleic anhydride surface, obtain the glass fibre reinforcement that multi-dimensional hybrid strengthens; Carbon nano-tube/nylon master batch is mixed with nylon resin, compound by the technique of extrusion moulding with above-mentioned glass fibre reinforcement again, obtain high-performance glass fiber reinforced nylon conducing composite material, in this matrix material, contain 30% glass fibre reinforcement and 5.3% carbon nano-tube/nylon master batch.
Step (1): in the beaker of 5L, add 6g ethene/copolymer-maleic anhydride and 3L deionized water, stir process 12h, obtains the aqueous solution of ethene/copolymer-maleic anhydride;
Step (2): take the carbon nanotube that 6g is dry, join in the aqueous solution of step (1) gained, process and stir 1h under the ultrasonic wave of 120kHz, obtain the suspension that carbon nanotube and ethene/copolymer-maleic anhydride coexist;
Step (3): take in the suspension that 600g commercialization glass fibre adds gained in step (2) to, stir process 20min, outwell supernatant liquid, repeatedly by washed with de-ionized water to remove the particle not being coated on glass fibre, 80 ℃ of dry 12h, obtain being coated with the multi-dimensional hybrid glass fibre reinforcement of carbon nanotube and ethene/copolymer-maleic anhydride;
Step (4): nylon resin is mixed with carbon nano-tube/nylon master batch, then with step (3) in the glass fibre reinforcement that mixes of gained by extruding-out process, undertaken compoundly, by following weight ratio, take material:
Nylon resin: 64.5 weight parts;
Multi-dimensional hybrid glass fibre reinforcement: 30 weight parts;
Carbon nano-tube/nylon master batch: 5.3 weight parts;
Oxidation inhibitor: 0.15～0.25 weight part;
Step (5): above-mentioned material is extruded and granulation through twin screw extruder, wherein glass fibre reinforcement is added by side feeding, extruder screw rotating speed is 120 revs/min, and temperature is 265 ℃, can obtain high-performance glass fiber reinforced polyamide conducing composite material.
Comparative example 1
Carbon nano-tube/nylon master batch is mixed with nylon resin, more compound by the technique of extrusion moulding with the commercialization glass fibre of not enveloped carbon nanometer tube and ethene/copolymer-maleic anhydride, obtain glass fibre reinforced nylon conducing composite material.
Step (1): take material by following weight percent content:
Nylon resin: 63.1%;
Glass fibre: 30%;
Carbon nano-tube/nylon master batch: 6.7%;
Oxidation inhibitor: 0.15～0.25%;
Step (2): above-mentioned material is extruded and granulation through twin screw extruder, and wherein glass fibre reinforcement is added by side feeding, and extruder screw rotating speed is 120 revs/min, and temperature is 265 ℃, obtains glass-fibre reinforced polyamide conducing composite material.
In embodiment 1～3 and comparative example 1, the nylon conducing composite material of preparation all contains 30% glass and 6.7% carbon nano-tube/nylon master batch.Embodiment 1～3 and comparative example 1 are carried out to the test of tensile strength, flexural strength, modulus in flexure, volume conductance and surface conductivity, and its test result is in Table 1.
From the measurement result to embodiment 1～3 and comparative example, the Mechanical Data of each embodiment and conduction data, all higher than comparative example, prove that its mechanics and conductivity are better than comparative example.
Claims (7)
1. a preparation method for high-performance glass fiber reinforced polyamide conducing composite material, is characterized in that, comprises the steps:
(1) take 1～20g ethene/copolymer-maleic anhydride, mix with the deionized water of 3～5L, in 10r/min～10
3r/min centrifugal speed stirs the lower 1～12h of processing, obtains the aqueous solution of ethene/copolymer-maleic anhydride;
(2) take the carbon nanotube that 2～20g is dry, add in the aqueous solution of described ethene/copolymer-maleic anhydride, in ultrasonic wave and 10r/min～10 of 60～120kHz
3r/min centrifugal speed stirs the lower 1～12h of processing, obtains the suspension that carbon nanotube and ethene/copolymer-maleic anhydride coexist;
(3) taking 10～1000g commercialization glass fibre adds in described suspension, in 10r/min～10
3under r/min centrifugal speed, stir the lower 1～60min of processing, outwell supernatant liquid, repeatedly by washed with de-ionized water to remove the particle not being coated on glass fibre, obtain the multi-dimensional hybrid glass fibre reinforcement of fiberglass surfacing enveloped carbon nanometer tube and ethene/copolymer-maleic anhydride after dry;
(4) nylon resin is mixed with carbon nano-tube/nylon master batch, then by extruding-out process, undertaken compound with described multi-dimensional hybrid glass fibre reinforcement; By following weight ratio, take material:
Nylon resin: 60～80 weight parts;
Multi-dimensional hybrid glass fibre reinforcement: 15～35 weight parts;
Carbon nano-tube/nylon master batch: 5～8 weight parts;
Oxidation inhibitor: 0.15～0.25 weight part;
(5) material after compound step (4) is extruded and granulation through twin screw extruder, wherein said multi-dimensional hybrid glass fibre reinforcement is added by side feeding, the screw speed of described twin screw extruder is 120～600 revs/min, temperature is 265～280 ℃, obtains described high-performance glass fiber reinforced polyamide conducing composite material.
2. preparation method according to claim 1, is characterized in that, described ethene/copolymer-maleic anhydride is poly-(ethene-alt-maleic anhydride).
3. preparation method according to claim 1, is characterized in that, described carbon nanotube is multi-walled carbon nano-tubes, and mean diameter is 10～20nm, and mean length is 3 μ m, and purity is greater than 90 % by weight.
4. preparation method according to claim 1, is characterized in that, described commercialization glass fibre is aminosilane coated glass fiber.
5. preparation method according to claim 1, is characterized in that, described nylon resin is nylon 6 or nylon 66, and wherein the fusing point of nylon 6 is 225 ℃, and the fusing point of nylon 66 is 265 ℃.
6. preparation method according to claim 1, is characterized in that, the formation of described carbon nano-tube/nylon master batch is: carbon nanotube: 15%, nylon master batch: 85%; The fusing point of described carbon nano-tube/nylon master batch is 263 ℃; Described carbon nanotube is multi-walled carbon nano-tubes, and described nylon master batch is nylon 66.
7. preparation method according to claim 1, is characterized in that, described oxidation inhibitor is the compound system of Hinered phenols antioxidant and phosphite ester kind antioxidant.
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Application publication date: 20130213 Assignee: JIANGSU XINGHE GROUP CO.,LTD. Assignor: EAST CHINA University OF SCIENCE AND TECHNOLOGY Contract record no.: X2022980011380 Denomination of invention: Preparation method of high performance glass fiber reinforced polyamide conductive composite Granted publication date: 20140430 License type: Exclusive License Record date: 20220728 |