CN108690350A - A kind of flame-retarded heat-conducting nylon plastic(s) and preparation method thereof that graphene is modified - Google Patents
A kind of flame-retarded heat-conducting nylon plastic(s) and preparation method thereof that graphene is modified Download PDFInfo
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- CN108690350A CN108690350A CN201710980543.8A CN201710980543A CN108690350A CN 108690350 A CN108690350 A CN 108690350A CN 201710980543 A CN201710980543 A CN 201710980543A CN 108690350 A CN108690350 A CN 108690350A
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- 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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
Abstract
The present invention provides the flame-retarded heat-conducting nylon plastic(s)s that a kind of graphene is modified, and include the ingredient of following mass fraction:High-fluidity nylon 6 is 44~72%;Negative ion powder 5~10%;Sulfonated graphene 5~10%;Spherical ceramic powder 1~3%;Polyamide elastomer 3~6%;Fire retardant 10~20%;Fire retarding synergist 3~5%;Processing aid 1~2%.Also disclose preparation method simultaneously.The flame-retarded heat-conducting nylon plastic(s) being modified using graphene prepared by the technology of the present invention, but also with flame retardant property while having high heat conduction, thermal coefficient reaches 5W/m. or more, flame retardant rating V-0.
Description
Technical field
The present invention relates to a kind of nylon composite materials, and in particular to a kind of flame-retarded heat-conducting nylon plastic(s) that graphene is modified and
Preparation method belongs to chemical material technical field.
Background technology
In recent years, with the development of industrial production and science and technology, great-power electronic, electric product are quickly sent out
There is the problems such as more and more causing product efficacy to reduce since product generates heat, reduced service life in exhibition.Data show that
Electronic component temperature often increases 2 DEG C, reliability decrease 10%;Service life at 50 DEG C only has 1/6 at 25 DEG C.
Nylon 6 is a kind of thermoplastic engineering plastic haveing excellent performance, have excellent mechanical property, preferable electrical property with
And it is wear-resisting, the advantages that oil resistant, solvent resistant, it is widely used in automobile, electronic apparatus, the fields such as machinery are especially led in LED illumination
Domain.But nylon 6 is heat insulation body, is used for a long time, and material temperature raising is easy to cause, and shadow is generated to the LED light service life
It rings.The heat filling such as aluminium oxide of the high additive amount of generally use at present, silicon nitride etc. carry out heat conduction modification, but this to nylon 6
Other performances of nylon, such as mechanical property and durability can be lost simultaneously.
Graphene is currently the nano material that most thin (single layer 0.335nm) is but also most hard in the world, it is almost complete
Transparent, it is seen that absorptivity is only 2.3%.The electron conduction of graphene is good, its electron mobility is higher than under room temperature
15000cm2/ V.s, and resistivity is only 10-6Ω cm are the material of current world resistivity minimum.Graphene is miscellaneous by sp2
Change carbon atom close-packed arrays to be formed, there is unique two-dimension periodic honeycomb lattice structure, it is steady in the presence of structural unit
Determine carbon hexatomic ring and assign its excellent hot property, it is considered to be outstanding heat control material.Graphene is added in nylon can pole
Big raising heat conductivity disclosure satisfy that heat management, electronics industry middle-high density, height by the high heat conduction plastics of filler of graphene
The requirement of integrated level assembling development.
Invention content
In view of the drawbacks of the prior art, the present invention provides a kind of excellent thermal conductivity, and machine-shaping is simple, and has excellent
Flame-retarded heat-conducting nylon plastic(s) of different flame retardant property and preparation method thereof.
The technical scheme is that:
A kind of flame-retarded heat-conducting nylon plastic(s) that graphene is modified, includes the ingredient of following mass fraction:
High-fluidity nylon 6 is 44~72%;Negative ion powder 5~10%;Sulfonated graphene 5~10%;Spherical ceramic powder
Body 1~3%;Polyamide elastomer 3~6%;Fire retardant 10~20%;Fire retarding synergist 3~5%;Processing aid 1~2%.
The negative ion powder is the compound of tourmaline powder and lanthanum chloride, and compounding mass ratio is 1:2~1:4.
Wherein, the size of the sulfonated graphene is 400nm~3 μm, 1~30nm of thickness, C in the sulfonated graphene
Molar ratio with S is 10:1~5:1;
Wherein, the relative viscosity of the high-fluidity nylon is 1.8~4.0dl/g;
Wherein, the spherical ceramic powder is one kind or combinations thereof in aluminium nitride, silicon nitride, four tungsten borides, grain size
For 200nm~500nm;
Wherein, the fire retardant is intumescent nano graphite flakes, and grain size is 1~5 μm;
Wherein, the fire retarding synergist be melamine cyanurate, melamine orthophosphate, it is a kind of in two melamine phosphates or
A combination thereof;
Wherein, the polyamide elastomer is the block copolymer of PA11 and PEO macromonomer;
Wherein, the processing aid is one kind or combinations thereof in antioxidant, nucleating agent, lubricant.
The present invention also provides the preparation methods for the flame-retarded heat-conducting nylon plastic(s) that the graphene is modified, and include the following steps:
1) various raw materials are weighed by above-mentioned formula;
2) by height flowing nylon 6 resin dry 1-2 hours at a temperature of 70 DEG C -80 DEG C, then with other all raw materials
It is uniformly mixed;
3) mixed raw material is placed in the lower hopper of extruder, is granulated through double screw extruder melting extrusion, you can obtain
Obtain the flame-retarded heat-conducting nylon plastic(s) that graphene is modified.
Further, the technological parameter of above-mentioned double screw extruder melting extrusion granulation is:One 190-195 DEG C of area's temperature,
Two 225-230 DEG C of area's temperature, three 230-235 DEG C of area's temperature, four 225-230 DEG C of area's temperature, five 220-225 DEG C of area's temperature, 6th area
205-210 DEG C of temperature, seven 210-215 DEG C of area's temperature, eight 210-215 DEG C of area's temperature, nine 220-225 DEG C of area's temperature, die head temperature
220-225℃;The rotating speed of host is 250-270r/min, and the rotating speed of feeding is 65-75r/min.
The present invention also provides the purposes for the flame-retarded heat-conducting nylon plastic(s) that the graphene is modified, and are used for automobile, electronics electricity
Device, mechanical device field are especially used for field of LED illumination.
The beneficial effects of the invention are as follows:
1) Buddhist nun is greatly improved by compounding the ingredients such as negative ion powder, sulfonated graphene, spherical ceramic powder in the present invention
The heat conductivility of dragon 6, thermal coefficient reach 5.0W/mK or more.In the present invention, the negative ion powder of use has higher negative
Ion generation amount and far infrared transmissivity, the heat given out using heat source can maintain the emissivities of negative ion powder, raising to lead
Hot nylon and extraneous energy exchange, to improve the heat dissipation effect of heat conduction nylon;Moreover, negative ion powder exists with sulfonated graphene
There is apparent synergistic effect on heat conductivility, the heat conductivility of material can be significantly increased.
2) present invention reaches V-0 grades by compounding intumescent nano graphite flakes and fire retarding synergist, the flame retardant rating of material
Not, and it is bittern-free flame-proof material;
Specific implementation mode
The present invention is illustrated in further details with reference to embodiments.It should be appreciated that the following example is only to show
Example property technical scheme of the present invention is explained and illustrated, and should not be used as the limitation to the application protection domain.
Unless otherwise indicated, the raw material in the following example is commercial product, or can be prepared by known method.
Specifically, the flame-retarded heat-conducting nylon plastic(s) that the graphene is modified, includes the ingredient of following mass fraction:
High-fluidity nylon 6 is 44~72%;Negative ion powder 5~10%;Sulfonated graphene 5~10%;Spherical ceramic powder
Body 1~3%;Polyamide elastomer 3~6%;Fire retardant 10~20%;Fire retarding synergist 3~5%;Processing aid 1~2%.
The negative ion powder is the compound of tourmaline powder and lanthanum chloride, and compounding mass ratio is 1:2~1:4.
Wherein, the size of the sulfonated graphene is 400nm~3 μm, 1~30nm of thickness, C in the sulfonated graphene
Molar ratio with S is 10:1~5:1;
Wherein, the relative viscosity of the high-fluidity nylon is 1.8~4.0dl/g;
Wherein, the spherical ceramic powder is one kind or combinations thereof in aluminium nitride, silicon nitride, four tungsten borides, grain size
For 200nm~500nm;
Wherein, the fire retardant is intumescent nano graphite flakes, and grain size is 1~5 μm;
Wherein, the fire retarding synergist be melamine cyanurate, melamine orthophosphate, it is a kind of in two melamine phosphates or
A combination thereof;
Wherein, the polyamide elastomer is the block copolymer of PA11 and PEO macromonomer;
Wherein, the processing aid is one kind or combinations thereof in antioxidant, nucleating agent, lubricant;
In the examples below that, the preparation method for the flame-retarded heat-conducting nylon plastic(s) that the graphene is modified includes following step
Suddenly:
1) various raw materials are weighed by above-mentioned formula;
2) by height flowing nylon 6 resin dry 1-2 hours at a temperature of 70 DEG C -80 DEG C, then with other all raw materials
It is uniformly mixed;
3) mixed raw material is placed in the lower hopper of extruder, is granulated through double screw extruder melting extrusion, you can obtain
Obtain the flame-retarded heat-conducting nylon plastic(s) that graphene is modified.
Further, the technological parameter of above-mentioned double screw extruder melting extrusion granulation is:One 190-195 DEG C of area's temperature,
Two 225-230 DEG C of area's temperature, three 230-235 DEG C of area's temperature, four 225-230 DEG C of area's temperature, five 220-225 DEG C of area's temperature, 6th area
205-210 DEG C of temperature, seven 210-215 DEG C of area's temperature, eight 210-215 DEG C of area's temperature, nine 220-225 DEG C of area's temperature, die head temperature
220-225℃;The rotating speed of host is 250-270r/min, and the rotating speed of feeding is 65-75r/min
Embodiment 1
A kind of flame-retarded heat-conducting nylon plastic(s) that graphene is modified, includes the ingredient of following mass fraction:
High-fluidity nylon 6 is 44%;Negative ion powder 10%;Sulfonated graphene 10%;Spherical ceramic powder 3%;Polyamides
Amine elastomer 6%;Fire retardant 20%;Fire retarding synergist 5%;Processing aid 2%.
Wherein, negative ion powder is the compound of tourmaline powder and lanthanum chloride, and compounding mass ratio is 1:2;Spherical ceramic powder
Body is aluminium nitride;Fire retarding synergist is melamine cyanurate, and processing aid is antioxidant.
It carries out preparing flame-retarded heat-conducting nylon plastic(s) as stated above.
Embodiment 2
A kind of flame-retarded heat-conducting nylon plastic(s) that graphene is modified, includes the ingredient of following mass fraction:
High-fluidity nylon 6 is 54.5%;Negative ion powder 8%;Sulfonated graphene 7%;Spherical ceramic powder 2%;Polyamides
Amine elastomer 5%;Fire retardant 18%;Fire retarding synergist 4%;Processing aid 1.5%.
Wherein, negative ion powder is the compound of tourmaline powder and lanthanum chloride, and compounding mass ratio is 1:3;Spherical ceramic powder
Body is silicon nitride;Fire retarding synergist is melamine orthophosphate, and processing aid is antioxidant and lubricant.
It carries out preparing flame-retarded heat-conducting nylon plastic(s) as stated above.
Embodiment 3
A kind of flame-retarded heat-conducting nylon plastic(s) that graphene is modified, includes the ingredient of following mass fraction:
High-fluidity nylon 6 is 72%;Negative ion powder 5%;Sulfonated graphene 5%;Spherical ceramic powder 1%;Polyamide
Elastomer 3%;Fire retardant 10%;Fire retarding synergist 3%;Processing aid 1%.
Wherein, negative ion powder is the compound of tourmaline powder and lanthanum chloride, compound proportion 1:4;Spherical ceramic powder is
Four tungsten borides;Fire retarding synergist is two melamine phosphates, and processing aid is antioxidant and lubricant.
It carries out preparing flame-retarded heat-conducting nylon plastic(s) as stated above.
The comparison of table 1 embodiment 1-3 and commercially available heat conduction nylon product performance
| Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 | Commercially available heat conduction nylon |
| Tensile strength MPa | 59.2 | 66.4 | 63.5 | 55.7 |
| Bending strength MPa | 95.4 | 97.8 | 96.1 | 90.3 |
| Thermal coefficient W/m.k | 6.1 | 5.5 | 5.1 | 1.8 |
| Notch impact strength KJ/m2 | 4.5 | 5.3 | 6.7 | 3.5 |
| Flame retardant rating (UL-94) | V-0 | V-0 | V-0 | V-0 |
As shown in Table 1, the modified heat-conduction nylon material of graphene of the present invention and heat conduction nylon product physical property phase on the market
Than thermal coefficient is significantly higher than general Heat Conduction Material on the market, and its mechanical strength is also very high, is more suitable for high power
LED seat etc. needs the electronic and electrical equipment of rapid cooling.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. the flame-retarded heat-conducting nylon plastic(s) that a kind of graphene is modified, includes the ingredient of following mass fraction:
High-fluidity nylon 6 is 44~72%;Negative ion powder 5~10%;Sulfonated graphene 5~10%;Spherical ceramic powder 1~
3%;Polyamide elastomer 3~6%;Fire retardant 10~20%;Fire retarding synergist 3~5%;Processing aid 1~2%.
2. the flame-retarded heat-conducting nylon plastic(s) that graphene as described in claim 1 is modified, which is characterized in that the negative ion powder is
For the compound of tourmaline powder and lanthanum chloride, compounding mass ratio is 1:2~1:4.
3. the flame-retarded heat-conducting nylon plastic(s) that graphene as claimed in claim 1 or 2 is modified, which is characterized in that the sulfonation
The size of graphene is 400nm~3 μm, and 1~30nm of thickness, the molar ratio of C and S is 10 in the sulfonated graphene:1~5:1.
4. the flame-retarded heat-conducting nylon plastic(s) that graphene as described in any one of claims 1-3 is modified, which is characterized in that the height
The relative viscosity of mobility nylon is 1.8~4.0dl/g.
5. the flame-retarded heat-conducting nylon plastic(s) that graphene according to any one of claims 1-4 is modified, which is characterized in that the ball
Shape ceramic powder is one kind or combinations thereof in aluminium nitride, silicon nitride, four tungsten borides;Preferably, the spherical ceramic powder
Grain size is 200nm~500nm.
6. the flame-retarded heat-conducting nylon plastic(s) that graphene as described in any one in claim 1-5 is modified, which is characterized in that described
Fire retardant is intumescent nano graphite flakes;Preferably, the grain size of the intumescent nano graphite flakes is 1~5 μm.
7. the flame-retarded heat-conducting nylon plastic(s) that graphene as claimed in any one of claims 1 to 6 is modified, which is characterized in that described
Fire retarding synergist is one kind or combinations thereof in melamine cyanurate, melamine orthophosphate, two melamine phosphates.
8. the flame-retarded heat-conducting nylon plastic(s) being modified such as claim 1-7 any one of them graphenes, which is characterized in that described
Polyamide elastomer is the block copolymer of PA11 and PEO macromonomer;
Preferably, the processing aid is one kind or combinations thereof in antioxidant, nucleating agent, lubricant.
9. such as the preparation method for the flame-retarded heat-conducting nylon plastic(s) that claim 1-8 any one of them graphenes are modified, including with
Lower step:
1) various raw materials are weighed by above-mentioned formula;
2) height flowing nylon 6 resin is 1-2 hours dry at a temperature of 70 DEG C -80 DEG C, then mixed with other all raw materials
Uniformly;
3) mixed raw material is placed in the lower hopper of extruder, is granulated through double screw extruder melting extrusion, you can obtain stone
The flame-retarded heat-conducting nylon plastic(s) that black alkene is modified;
Preferably, the technological parameter of above-mentioned double screw extruder melting extrusion granulation is:One 190-195 DEG C of area's temperature, two area's temperature
225-230 DEG C of degree, three 230-235 DEG C of area's temperature, four 225-230 DEG C of area's temperature, five 220-225 DEG C of area's temperature, six area's temperature
205-210 DEG C, seven 210-215 DEG C of area's temperature, eight 210-215 DEG C of area's temperature, nine 220-225 DEG C of area's temperature, die head temperature 220-
225℃;The rotating speed of host is 250-270r/min, and the rotating speed of feeding is 65-75r/min.
10. such as the purposes for the flame-retarded heat-conducting nylon plastic(s) that claim 1-8 any one of them graphenes are modified, it to be used for vapour
Vehicle, electronic apparatus, mechanical device field are especially used for field of LED illumination.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710980543.8A CN108690350A (en) | 2017-10-19 | 2017-10-19 | A kind of flame-retarded heat-conducting nylon plastic(s) and preparation method thereof that graphene is modified |
| CN201811204391.3A CN109354868B (en) | 2017-10-19 | 2018-10-16 | Graphene-modified flame-retardant heat-conducting nylon plastic and preparation method thereof |
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| CN201710980543.8A CN108690350A (en) | 2017-10-19 | 2017-10-19 | A kind of flame-retarded heat-conducting nylon plastic(s) and preparation method thereof that graphene is modified |
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| CN201811204391.3A Active CN109354868B (en) | 2017-10-19 | 2018-10-16 | Graphene-modified flame-retardant heat-conducting nylon plastic and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109608875A (en) * | 2019-01-10 | 2019-04-12 | 厦门大学 | A kind of thermally conductive nylon 6 resin composite material and preparation method |
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| US20150232664A1 (en) * | 2012-09-07 | 2015-08-20 | Sabic Innovative Plastics Ip B.V. | Thermally conductive blended polymer compositions with improved flame retardancy |
| CN103819735B (en) * | 2014-03-03 | 2016-03-02 | 中国科学院青岛生物能源与过程研究所 | Expansible black lead/melamine salt synergistic expanding fire retardant and preparation method thereof |
| CN104844794B (en) * | 2015-05-20 | 2017-05-31 | 苏州高通新材料科技有限公司 | Heat-conduction nylon material based on sulfonated graphene and preparation method thereof |
| CN105462246B (en) * | 2015-12-30 | 2018-04-06 | 广东聚石化学股份有限公司 | Powder compound modified super-high heat-conductive nylon of a kind of graphene/metal and preparation method thereof |
| CN105820557B (en) * | 2016-04-25 | 2019-02-01 | 惠州市环美盛新材料有限公司 | A kind of flame-retarded heat-conducting nylon and preparation method thereof |
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| CN109608875A (en) * | 2019-01-10 | 2019-04-12 | 厦门大学 | A kind of thermally conductive nylon 6 resin composite material and preparation method |
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Application publication date: 20181023 |