CN103951974A - Anti-static heat-conducting nylon composite material and preparation method for same - Google Patents

Anti-static heat-conducting nylon composite material and preparation method for same Download PDF

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Publication number
CN103951974A
CN103951974A CN201410205416.7A CN201410205416A CN103951974A CN 103951974 A CN103951974 A CN 103951974A CN 201410205416 A CN201410205416 A CN 201410205416A CN 103951974 A CN103951974 A CN 103951974A
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nylon
parts
conducting
whisker
electrostatic
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CN103951974B (en
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姚大虎
刘任晖
刘成
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PINGDINGSHAN HUABANG ENGINEERING PLASTIC Co Ltd
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PINGDINGSHAN HUABANG ENGINEERING PLASTIC Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/06—Elements
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/08—Oxygen-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/04—Antistatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group

Abstract

The invention belongs to the field of organic polymer composite materials, and particularly relates to an anti-static heat-conducting nylon composite material and a preparation method for the same. The composite material is prepared from the following raw materials in parts by mass: 50-100 parts of nylon resin, 5-30 parts of carbon fibres, 1-10 parts of expanded graphite, 5-20 parts of high-heat-conductivity crystal whisker filler, 0.5-2 parts of coupling agent and 0.5-5 parts of antioxidant, wherein the materials above are mixed and extruded by a double-screw extruder at a high temperature to obtain the nylon composite material which is low in the dosage of carbon fibres, and good in electricity-conducting and heat-conducting effects. According to the composite material and the preparation method for the same disclosed by the invention, an interconnected 'micro-network' is formed by mutually cooperating the lamellar structure of graphene and the acicular structure of the fine heat-conducting filler, and the 'micro-network' is communicated with the carbon fibres penetrating through the composite material to form a channel with good electricity-conducting and heat-conducting effects, thus acting good electricity-conducting and heat-conducting effects, and reducing the dosage of the carbon fibres simultaneously.

Description

A kind of electrostatic-resistant heat conducting nylon composite materials and preparation method thereof
Technical field
The invention belongs to organic polymer composite field, relate in particular to a kind of electrostatic-resistant heat conducting nylon composite materials and preparation method thereof.
Background technology
Nylon resin is excellent performance, broad-spectrum industrial chemicals, and the characteristic such as, light weight nontoxic owing to having, wear-resisting, corrosion-resistant and good mechanical property, is therefore widely used in the industrial circles such as machinery, automobile, chemical industry, instrument.Nylon resin has very high surface resistivity, in use because friction is easy to, at surperficial stored charge, cause static discharge, produces electrical spark and cause fire.People improve electrical property and the heat conductivility of polymkeric substance conventionally by adding the method for conductive filler material, but give the desirable conductivity of nylon resin and heat conductivility and need to fill a large amount of conductive filler materials, can cause like this moulding processability of matrix material and the significantly decline of mechanical property.Antistatic and the Heat Conduction Problems that how to solve in recent years nylon resin has caused and has shown great attention in polymer composite field.
Carbon fiber has that high specific strength, high ratio modulus, high temperature resistant, conduction are conducted heat and the advantage such as thermal expansivity is little.Therefore can play the effect of conduction, heat conduction and enhancing by add carbon fiber in nylon resin simultaneously.But in the time using carbon fiber as conductive filler material, must make to interconnect between carbon fiber as need make polymkeric substance have good electroconductibility, form conductive path.The add-on of carbon fiber is larger like this, can increase substantially cost.
Summary of the invention
The object of this invention is to provide a kind of electrostatic-resistant heat conducting nylon composite materials and preparation method thereof, carbon fiber consumption of the present invention is few, has high conduction, high thermal conductivity.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of electrostatic-resistant heat conducting nylon composite materials, is made up of following mass parts raw material: nylon resin 50-100 part, carbon fiber 5-30 part, expanded graphite 1-10 part, high heat conduction whisker filler 5-20, coupling agent 0.5-2 part and oxidation inhibitor 0.5-5 part.
Described electrostatic-resistant heat conducting nylon composite materials, its raw material preferred mass umber is: nylon resin 70-90 part, carbon fiber 10-20 part, expanded graphite 5-10 part, high heat conduction whisker filler 10-20, coupling agent 1-2 part and oxidation inhibitor 0.5-1 part.
Preferably, described high heat conduction whisker filler preparation method is as follows: get and anyly in calcium carbonate crystal whisker, ZnOw or alumina whisker mix with water, then add SnCl 4, the pH value of regulation system was 9-10,70 DEG C of reactions 60 minutes; Dry after filtering, then within 3-4 hour, obtain described high heat conduction whisker filler, calcium carbonate crystal whisker or ZnOw or alumina whisker, water and SnCl 600-700 DEG C of calcining 4quality proportioning be 10:25-50:1-3.5, the ammoniacal liquor that described pH adjusting agent is 0.1mol/L or the sodium hydroxide of 0.1mol/L.
Preferably, described nylon resin is nylon 6, nylon 66 or both mixtures.
Preferably, described coupling agent is silane coupling agent or titante coupling agent.
A preparation method for electrostatic-resistant heat conducting nylon composite materials, step is as follows:
1) get respectively each raw material by mass parts, by nylon resin, expanded graphite and high heat conduction whisker filler heat drying respectively, then after stirring in high-speed mixer with coupling agent and oxidation inhibitor, send into twin screw extruder, then carbon fiber is added twin screw extruder from the side spout of twin screw extruder;
2) twin screw extruder is not less than to 0.07MPa in vacuum tightness, under the condition of 175 DEG C-275 DEG C, mixture is extruded, and then through tie rod, cooling, pelletizing and dry, obtain described electrostatic-resistant heat conducting nylon composite materials.
The present invention at Double-screw forcing machine in the time that nylon resin and carbon fiber are carried out to high temperature extrusion, high temperature can make nylon resin intercalation in expanded graphite, in nylon resin, forming graphene nano lamella disperses, and Graphene has good electroconductibility, the high heat conduction whisker filler of needle-like disperses to form wire in nylon, Graphene plays bridged linkage, mutually collaborative with high heat conduction whisker filler, forms ' micronetwork ' with heat conduction, conductivity; ' micronetwork ' is mutually collaborative with the distribution of carbon fiber, plays good conduction, heat-conducting effect, can fully reduce the consumption of carbon fiber, reduces the preparation cost of raw material.
The present invention compared with prior art, tool has the following advantages: utilize the laminated structure of Graphene and the acicular structure of meticulous shape heat conductive filler, collaborative formation interconnective ' micronetwork ' mutually, be somebody's turn to do ' microcosmos network ' and be interconnected through the carbon fiber of matrix material, form conduction, thermal conducting path preferably, play good conduction, heat-conducting effect, reduced the consumption of carbon fiber simultaneously.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with specific embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
embodiment 1:
Get respectively 1 part, 50 parts of Nylon 66s, 10 parts, carbon fiber, 10 parts of expanded graphites, 5 parts of high heat conduction whisker fillers, 0.5 part of coupling agent and oxidation inhibitor by mass parts;
Described high heat conduction whisker filler preparation method is as follows: get calcium carbonate crystal whisker and mix with water, then add SnCl 4, using the pH value of pH adjusting agent regulation system was 9,70 DEG C of reactions 60 minutes; Dry after filtering, then within 3 hours, obtain described high heat conduction whisker filler, calcium carbonate crystal whisker, water and SnCl 600 DEG C of calcinings 4quality proportioning be 10:25:1, pH adjusting agent is 0.1mol/L ammoniacal liquor.
By Nylon 66, expanded graphite and high heat conduction whisker filler heat drying respectively, then after stirring in high-speed mixer with coupling agent and oxidation inhibitor, send into twin screw extruder, then carbon fiber is added twin screw extruder from the side spout of twin screw extruder; By twin screw extruder, at vacuum tightness 0.07MPa, temperature is extruded mixture under the condition of 175 DEG C, and then through tie rod, cooling, pelletizing and dry, obtains described electrostatic-resistant heat conducting nylon composite materials
embodiment 2:
Get respectively 0.5 part, 50 parts of Nylon 66s, 5 parts, carbon fiber, 1 part of expanded graphite, 20 parts of high heat conduction whisker fillers, 0.5 part of coupling agent and oxidation inhibitor by mass parts;
Described high heat conduction whisker filler preparation method is as follows: get ZnOw and mix with water, then add SnCl 4, using the pH value of pH adjusting agent regulation system was 10,70 DEG C of reactions 60 minutes; Dry after filtering, then within 4 hours, obtain described high heat conduction whisker filler, ZnOw, water and SnCl 700 DEG C of calcinings 4quality proportioning be 10:25:3.5, pH adjusting agent is 0.1mol/L sodium hydroxide solution.
By Nylon 66, expanded graphite and high heat conduction whisker filler heat drying respectively, then after stirring in high-speed mixer with coupling agent and oxidation inhibitor, send into twin screw extruder, then carbon fiber is added twin screw extruder from the side spout of twin screw extruder; By twin screw extruder, at vacuum tightness 0.08MPa, temperature is extruded mixture under the condition of 275 DEG C, and then through tie rod, cooling, pelletizing and dry, obtains described electrostatic-resistant heat conducting nylon composite materials
embodiment 3:
Get respectively 2 parts, 100 parts of Nylon 66s, 30 parts, carbon fiber, 5 parts of expanded graphites, 10 parts of high heat conduction whisker fillers, 2 parts of coupling agents and oxidation inhibitor by mass parts;
Described high heat conduction whisker filler preparation method is as follows: get alumina whisker and mix with water, then add SnCl 4, the pH value of regulation system was 10,70 DEG C of reactions 60 minutes; Dry after filtering, then within 3 hours, obtain described high heat conduction whisker filler, alumina whisker, water and SnCl 700 DEG C of calcinings 4quality proportioning be 10:50:3.5, pH adjusting agent is 0.1mol/L ammoniacal liquor.
By Nylon 66, expanded graphite and high heat conduction whisker filler heat drying respectively, then after stirring in high-speed mixer with coupling agent and oxidation inhibitor, send into twin screw extruder, then carbon fiber is added twin screw extruder from the side spout of twin screw extruder; Twin screw extruder, at vacuum tightness 0.07MPa, under the condition that temperature is 275 DEG C is extruded mixture, and then through tie rod, cooling, pelletizing and dry, obtained described electrostatic-resistant heat conducting nylon composite materials
embodiment 4:
Get respectively 1 part, 80 parts of Nylon 6s, 15 parts, carbon fiber, 3 parts of expanded graphites, 15 parts of high heat conduction whisker fillers, 1 part of coupling agent and oxidation inhibitor by mass parts;
Described high heat conduction whisker filler preparation method is as follows: get alumina whisker and mix with water, then add SnCl 4, the pH value of regulation system was 10,70 DEG C of reactions 60 minutes; Dry after filtering, then within 4 hours, obtain described high heat conduction whisker filler, alumina whisker, water and SnCl 600 DEG C of calcinings 4quality proportioning be 10:50:3.5, pH adjusting agent is 0.1mol/L ammoniacal liquor.
By Nylon 6, expanded graphite and high heat conduction whisker filler heat drying respectively, then after stirring in high-speed mixer with coupling agent and oxidation inhibitor, send into twin screw extruder, then carbon fiber is added twin screw extruder from the side spout of twin screw extruder; By twin screw extruder, at vacuum tightness 0.07MPa, temperature is extruded mixture under the condition of 175 DEG C, and then through tie rod, cooling, pelletizing and dry, obtains described electrostatic-resistant heat conducting nylon composite materials.
embodiment 5:
Get respectively 1 part, 45 parts of Nylon 66s, 45 parts of Nylon 6s, 20 parts, carbon fiber, 10 parts of expanded graphites, 10 parts of the high heat conduction whisker of calcium carbonate-base fillers, 1 part of coupling agent and oxidation inhibitor by mass parts;
Described high heat conduction whisker filler preparation method is as follows: get ZnOw and mix with water, then add SnCl 4, the pH value of regulation system was 10,70 DEG C of reactions 60 minutes; Dry after filtering, then within 3.5 hours, obtain described high heat conduction whisker filler, ZnOw, water and SnCl 650 DEG C of calcinings 4quality proportioning be 10:25:1, pH adjusting agent is 0.1mol/L ammoniacal liquor.
By Nylon 66, Nylon 6, expanded graphite and high heat conduction whisker filler heat drying respectively, then after stirring in high-speed mixer with coupling agent and oxidation inhibitor, send into twin screw extruder, then carbon fiber is added twin screw extruder from the side spout of twin screw extruder; By twin screw extruder, at vacuum tightness 0.07MPa, temperature is extruded mixture under the condition of 175 DEG C, and then through tie rod, cooling, pelletizing and dry, obtains described electrostatic-resistant heat conducting nylon composite materials.
Performance test and result:
Testing method: surface resistivity test is pressed ASTMD257 standard and carried out, ASTMD638 operative norm is pressed in tensile strength and elongation at break test, and flexural strength and modulus test are pressed ASTMD790 standard and are carried out, and notched Izod impact strength is carried out according to ASTMD256 standard; Test result refers to table one
Table one
? Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5
Tensile strength/MPa 160 174 182 164 172
Elongation at break/% 7 5 4 7 4
Flexural strength/MPa 241 254 270 246 261
Bending elastic modulus/MPa 14400 15200 16100 14700 15600
Notched Izod impact strength/KJ/m 2 27 31 28 36 33
Volume specific resistance/Ω cn 72 83 95 76 81
Thermal conductivity/W/mK 3.1 2.9 2.7 3.0 3.1

Claims (6)

1. an electrostatic-resistant heat conducting nylon composite materials, it is characterized in that, made by following mass parts raw material: nylon resin 50-100 part, carbon fiber 5-30 part, expanded graphite 1-10 part, high heat conduction whisker filler 5-20, coupling agent 0.5-2 part and oxidation inhibitor 0.5-5 part.
2. a kind of electrostatic-resistant heat conducting nylon composite materials as claimed in claim 1, it is characterized in that, made by following mass parts raw material: nylon resin 70-90 part, carbon fiber 10-20 part, expanded graphite 5-10 part, high heat conduction whisker filler 10-20, coupling agent 1-2 part and oxidation inhibitor 0.5-1 part.
3. a kind of electrostatic-resistant heat conducting nylon composite materials as claimed in claim 1 or 2, it is characterized in that, described high heat conduction whisker filler preparation method is as follows: get and anyly in calcium carbonate crystal whisker, ZnOw or alumina whisker mix with water, then add SnCl 4, the pH value of regulation system was 9-10,70 DEG C of reactions 60 minutes; Dry after filtering, then within 3-4 hour, obtain described high heat conduction whisker filler, calcium carbonate crystal whisker or ZnOw or alumina whisker, water and SnCl 600-700 DEG C of calcining 4quality proportioning be 10:25-50:1-3.5, the ammoniacal liquor that described pH adjusting agent is 0.1mol/L or the sodium hydroxide of 0.1mol/L.
4. a kind of electrostatic-resistant heat conducting nylon composite materials as claimed in claim 1 or 2, is characterized in that, described nylon resin is nylon 6, nylon 66 or both mixtures.
5. a kind of electrostatic-resistant heat conducting nylon composite materials as claimed in claim 1 or 2, is characterized in that, described coupling agent is silane coupling agent or titante coupling agent.
6. the preparation method of a kind of electrostatic-resistant heat conducting nylon composite materials described in claim 1 or 2, is characterized in that, step is as follows:
1) get respectively each raw material by mass parts, by nylon resin, expanded graphite and high heat conduction whisker filler heat drying respectively, then after stirring in high-speed mixer with coupling agent and oxidation inhibitor, send into twin screw extruder, then carbon fiber is added twin screw extruder from the side spout of twin screw extruder;
2) twin screw extruder is not less than to 0.07MPa in vacuum tightness, under the condition of 175 DEG C-275 DEG C, mixture is extruded, and then through tie rod, cooling, pelletizing and dry, obtain described electrostatic-resistant heat conducting nylon composite materials.
CN201410205416.7A 2014-05-15 2014-05-15 A kind of electrostatic-resistant heat conducting nylon composite materials and its preparation method Expired - Fee Related CN103951974B (en)

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CN104559149A (en) * 2014-12-16 2015-04-29 惠州力王佐信科技有限公司 Carbon composite high-thermal-conductivity plastic material and preparation method thereof
CN104559146A (en) * 2014-12-16 2015-04-29 惠州力王佐信科技有限公司 Whisker reinforced thermally conductive plastic material and preparation method thereof
CN104845358A (en) * 2015-04-17 2015-08-19 柳州蔚园塑料彩印包装有限责任公司 High strength engineering plastic
CN104893100A (en) * 2015-05-29 2015-09-09 安徽顺彤包装材料有限公司 Anti-explosion and anti-electrostatic material and preparation method thereof
CN105295360A (en) * 2015-10-10 2016-02-03 惠州市沃特新材料有限公司 High thermal conductivity flame-retardant nylon composite material and preparation method thereof
CN105778494A (en) * 2016-03-08 2016-07-20 苏州珍展科技材料有限公司 Preparation method of polyamide and carbon fiber composite material
CN106084760A (en) * 2016-06-22 2016-11-09 中北大学 A kind of nylon 6/ thermal expansion graphite conducting composite material and preparation method thereof
CN106867243A (en) * 2015-12-11 2017-06-20 上海杰事杰新材料(集团)股份有限公司 A kind of antistatic high temperature resistant nylon composite material of high heat conduction and preparation method thereof
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CN107629355A (en) * 2017-09-22 2018-01-26 扬州大学 A kind of preparation method of antistatic herd polyvinyl chloride material
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CN104559146A (en) * 2014-12-16 2015-04-29 惠州力王佐信科技有限公司 Whisker reinforced thermally conductive plastic material and preparation method thereof
CN104559149A (en) * 2014-12-16 2015-04-29 惠州力王佐信科技有限公司 Carbon composite high-thermal-conductivity plastic material and preparation method thereof
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