CN103483809A - High-flowability polyamide based halogen-free flame-retardant heat-conducting composite material and preparation method thereof - Google Patents
High-flowability polyamide based halogen-free flame-retardant heat-conducting composite material and preparation method thereof Download PDFInfo
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- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
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Abstract
The invention discloses a high-flowability polyamide halogen-free flame-retardant heat-conducting composite material and a preparation method thereof. A novel halogen-free flame-retardant heat-conducting composite material is prepared by using high-flowability nylon 6 resin with a branch chain structure as a base body, adding additives such as heat-conducting fillers, a halogen-free flame retardant, an antioxidant and a coupler, and preparing the material through a double-screw melt blending technology. The halogen-free flame-retardant heat-conducting composite material has the characteristics of good heat conductivity, high melt flowability, good environment-friendly and flame-retardant performances, excellent insulation and mechanical comprehensive performances and the like; an obtained product is high in heat-radiating speed, high in strength, low in warping degree and resistant to high temperature and ageing; the composite material can be widely applied to the field of electric plastic parts with higher heat-radiating requirements such as locomotive compartment illumination lamp covers, auto and civil LED heat radiators, household appliance motor shells, notebook power, micro-projector shells, transformer coil frameworks and the like.
Description
Technical field
The present invention relates to a kind of high-fluidity polyamide base halogen-free flame-retarded heat-conducting matrix material and preparation method thereof.
Background technology
Polyamide compoiste material is widely used in the fields such as electronic apparatus, mechanical means because of excellent over-all properties, this type component has been played the part of the role of structural part and functional part simultaneously.Development trend along with electronics lightweight and miniaturization, Electronic Assemblies density improves rapidly, the heat that requires components and parts to produce in the course of the work must distribute in time and conduct, otherwise have influence on the work-ing life of system energy efficiency utilization and goods, thereby the heat conductivility of material is had higher requirement.But the thermal conductivity of polymeric amide is only 0.23W/ (m.K), far can not meet the requirement of functional type heat-conducting plastic, the heat conductivility that therefore improves polyamide compoiste material has practical significance.
The main method for preparing at present heat-conducting plastic is to filling high heat conduction component in polymeric matrix, by the interaction between heat conductive filler, forms similar chain or netted distributional pattern in system---heat conduction network chain and improve the thermal conductivity of matrix material.The metal oxide-type heat conductive filler is because of its good insulation preformance, the low first-selection for preparing filled-in composite that becomes of cost, but the preparation method exists following difficulty and defect: be because the capacity of heat transmission of metal oxide-type heat conductive filler own is limited on the one hand, when filler content is low, the matrix material thermal conductivity does not reach requirement, and filler content is when too high (being greater than 70 wt %), the fluidity of molten of matrix material is too poor and can't process; Because heat conductive filler is inorganic materials on the other hand, bad with the consistency of macromolecular material matrix, cause the mechanical properties decrease of matrix material obvious, and interface resistance has hindered the raising of thermal conductivity.Simultaneously, consider that thermally conductive material contacts with thermal source for a long time, must take into account heat-resisting, ageing resistance and the flame retardant properties of matrix material.Therefore, how when improving the matrix material thermal conductivity, to keep the over-all properties of matrix resin excellence to become the important directions that heat-conductive composite material is studied.
Patent " flame-retarded heat-conducting nylon 66 composite material and preparation method thereof " open (bulletin) number-: CN102399442A be take conventional PA66 as matrix, its heat conductive filler is metal nitride and conductive powder, pass through double-screw extruding pelletizing, because of conventional PA66 fluidity of molten limited, loading level and the distribution of filler in matrix of filler in this matrix material have seriously been limited, affect the formation of heat conduction network chain, caused the capacity of heat transmission of matrix material limited; The mobility of matrix material is poor, affects Drawing abillity and products appearance.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of high-fluidity polyamide base halogen-free flame-retarded heat-conducting matrix material.This material can be widely used in the Electric Plastic part field that the heat radiations such as railway locomotive railway carriage illuminating lamp shade, automobile and civil LED scatterer, household electrical appliances motor housing, laptop, micro-shape projector case, transformer coil frame are had relatively high expectations.
Another technical problem that will solve of the present invention is to provide the preparation method of above-mentioned halogen-free flame-retarded heat-conducting nylon composite materials.Adopt that halogen-free flame-retarded heat-conducting nylon composite materials prepared by this technology has that thermal conductivity is high, fluidity of molten good, insulating property are good, the characteristics such as mechanical property and flame retardant properties excellence.
In order to solve the problems of the technologies described above, the present invention relates to a kind of high-fluidity polyamide base halogen-free flame-retarded heat-conducting matrix material its, this matrix material is composed of the following components by weight percentage:
Nylon resin: 5-85;
Heat conductive filler: 10-80;
Halogen-free flame retardants: 1-15;
Oxidation inhibitor: 0.1-0.5;
Coupling agent: 0.1-2;
Further, described nylon resin is a kind of at least containing the high-fluidity nylon composition of branched structure nylon 6, is high-fluidity nylon 6 and nylon 6, nylon 66, nylon 46, nylon 12, nylon 612, the arbitrary combination of nylon 1212 and aromatic nylon.Described high-fluidity nylon 6 resins are that branching unit initiator and hexanolactam prepare by hydrolytic polymerization.Described high-fluidity nylon 6 resins are 230 in shear temperature
oC, shearing resistance is 500s
-1under condition, relative viscosity is 1.1-2.8, and kinematic viscosity is between 10Pa.s-1000 Pa.s.
Described heat conductive filler component is a kind of or arbitrary combination in magnesium oxide, magnesium nitride, ball-aluminium oxide, class ball-aluminium oxide, aluminium nitride, boron nitride, pitch fibers, halloysite, carbon nanotube, graphite, silicon carbide, boehmite.
Described halogen-free flame retardants comprises a kind of or arbitrary combination of the agent of phosphorus nitrogen fire-retardant, the agent of alkylphosphonic fire-retardant and inorganic fire-retardant agent.Wherein, the agent of phosphorus nitrogen fire-retardant is a kind of or arbitrary combination of trimeric cyanamide-poly-phosphate (MP), trimeric cyanamide-polyphosphoric acid salt (MP) and trimeric cyanamide-focusing phosphoric acid salt; The agent of alkylphosphonic fire-retardant is a kind of or arbitrary combination of alkyl hypophosphite, alkyl metaphosphate or alkyl phosphite; Inorganic fire-retardant agent comprises ammonium polyphosphate (APP), aluminium hydroxide, magnesium hydroxide, expanded polystyrene veneer graphite, sal epsom seven water and molybdenum oxide is a kind of or arbitrary combination.
The arbitrary combination that described oxidation inhibitor is Hinered phenols antioxidant and phosphite ester kind antioxidant.
A kind of or the arbitrary combination that described coupling agent is silane coupling agent (KH792, KH550, KH560, KH570) or epoxy group(ing) aliphatic polyester.
The preparation method of high-fluidity polyamide base halogen-free flame-retarded heat-conducting matrix material is characterized in that this preparation method comprises following processing step:
(1) heat conductive filler, coupling agent are joined in high-speed mixer and fully mix;
(2) all mixed things that step (1) obtained join in mixing machine and fully mix with nylon resin, fire retardant, oxidation inhibitor;
(3) all mixed things that step (2) obtained melt extrude by screw extrusion press, through traction, cooling, pelletizing, obtain high-fluidity polyamide base halogen-free flame-retarded heat-conducting matrix material.
The temperature at the barrel rear portion of described forcing machine is that 220 ℃-250 ℃, the temperature at barrel middle part are that 250 ℃-280 ℃, the temperature of barrel front portion are that 270 ℃-280 ℃, nozzle temperature are 275 ℃-280 ℃; Screw speed is 180-350r/min; Rate of feeding is 10-20r/min.
By institute's granulation in vacuum drying oven under 100 ℃ of-120 ℃ of conditions dry 4-8h.
Also comprise Shooting Technique after described granulating and drying, the temperature at injecting machine material tube rear portion is that 250 ℃-270 ℃, the temperature at barrel middle part are that 270 ℃-290 ℃, the temperature of barrel front portion are 290 ℃-295 ℃; Nozzle temperature is 295 ℃-300 ℃; Die temperature is 80 ℃-100 ℃; Screw speed is 100-120r/min; The injection back pressure is 60-80Mpa.
Described high workability halogen-free flame-retarded heat-conducting nylon composite materials can be used for following processing mode: molded, injection molding, extrusion moulding.
Described high workability halogen-free flame-retarded heat-conducting nylon composite materials can be used for the Electric Plastic part field that the heat radiations such as LED scatterer, stepper-motor shell, laptop, micro-shape projector case, transformer coil frame are had relatively high expectations.
With existing technology of preparing, compare, introduced the side chain Nylon 6 of high fluidity of molten and a large amount of active end groups in technology of preparing of the present invention, effectively promoted dispersion, the processing characteristics of having improved high filling nylon composite material, the dipping that improved fire retardant and the consistency of heat conductive filler in matrix, make filling components and fire retardant fully coat and be dispersed in matrix resin, thereby the present invention has following advantage:
1, excellent heat conductivility, heat transfer property and high thermal diffusivity.
2, high, the halogen-free environmental of flame retarding efficiency, low flame radiation, smoke density are low.
3, good insulation preformance, mechanical property are excellent, high temperature resistant, ageing-resistant.
4, low, the good stability of the dimension of molding shrinkage, low warpage, high-flatness.
5, fluidity of molten excellent, be easy to processing; Recipe is simple, workable, suitability is wide.
Embodiment
Below the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, embodiments of the invention are including, but not limited to described embodiment.Based on this, those skilled in the art, not making under the innovative works prerequisite the every other embodiment obtained, all belong to the scope that the present invention protects.
In inventive embodiments, the resin that adopts is Dendritic Nylon or ultra-branching nylon, and what in the comparative example, adopt is conventional nylon, and the embodiment of the present invention and comparison example see the following form 1:
Table 1 embodiment and comparison example material formula table
Wherein, in shear temperature, be 230
oC, shearing resistance is 500s
-1under test condition, dendroid type high-fluidity nylon 6 relative viscosities are 1.6; Hyperbranched type high-fluidity nylon 6 relative viscosities are 1.7.
As shown in table 1 is the material formula table of embodiment and comparison example, is below the preparation method of embodiment and comparison example:
(1) heat conductive filler, coupling agent are joined in high-speed mixer and fully mix;
(2) all mixed things that step (1) obtained join in mixing machine and fully mix with nylon resin, fire retardant, oxidation inhibitor;
(3) all mixed things that step (2) obtained melt extrude by screw extrusion press, through traction, cooling, pelletizing, obtain high workability halogen-free flame-retarded heat-conducting nylon composite materials.
(4) high workability halogen-free flame-retarded heat-conducting nylon composite materials is made the standard batten through injection moulding and is detected.
For embodiment 1,2,3,4 and comparison example 1,2,3,4 carry out a series of tests such as heat conductivility, mechanical property, flame retardant properties and appearance, test result is as shown in table 2.
The material properties test result of table 2 embodiment and comparison example
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparison example 1 | Comparison example 2 | Comparison example 3 | Comparison example 4 |
| MFI（g/10min） | 28.1 | 23.8 | 16.4 | 11.5 | 12.4 | 10.7 | 6.9 | 4.7 |
| Lateral shrinkage (%) | 0.23 | 0.22 | 0.23 | 0.21 | 0.28 | 0.27 | 0.29 | 0.285 |
| Longitudinal contraction rate (%) | 0.3 | 0.323 | 0.3 | 0.32 | 0.38 | 0.4 | 0.38 | 0.39 |
| Vertical direction thermal conductivity (W/m.k -1） | 1.35 | 1.78 | 1.52 | 1.82 | 1.16 | 1.23 | 1.15 | 1.17 |
| Tensile strength (Mpa) | 74 | 71.5 | 78 | 73.2 | 70 | 68 | 71 | 70 |
| Flexural strength (Mpa) | 101 | 106 | 109 | 111 | 88 | 91 | 93 | 96 |
| Modulus in flexure (Mpa) | 8600 | 8800 | 9000 | 9100 | 8700 | 8800 | 8900 | 8900 |
| Simply supported beam notched Izod impact strength (KJ/m2) | 5.8 | 5.2 | 6.6 | 5.4 | 4.4 | 3.9 | 4.6 | 4.1 |
| Simply supported beam unnotched impact strength (KJ/m2) | 13.6 | 11.2 | 15.3 | 11.8 | 10.9 | 9.6 | 11.3 | 10.8 |
| Heat-drawn wire (℃) | 176 | 178 | 182 | 185 | 171 | 174 | 179 | 182 |
| UL94(3.2mm) | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 |
| UL94(1.6mm) | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 | V-1 | V-1 |
| UL94(0.8mm) | V-0 | V-0 | V-1 | V-1 | V-1 | V-1 | V-2 | V-2 |
| Appearance | Good | Good | Good | Good | Generally | Generally | Generally | Poor |
Wherein, the test condition of melting index (MFI) is 275 ℃/2.16kg; The Determination of conductive coefficients instrument is Hot Disk, and testing standard is ISO-DIS22007; The heat-drawn wire testing standard is: GB/T 1634-2004(0.45MPa, B method).
Consolidated statement 1 and table 2 are visible, with comparison example 1, 2, 3, 4 compare, the invention process example 1, 2, 3, the fluidity of molten of the high workability halogen-free flame-retarded heat-conducting nylon composite materials in 4 has all improved nearly 3 times, significantly improved the processing characteristics of high filled composite materials, promoted filler simultaneously, the formation of heat conduction network chain in the dispersion of fire retardant in matrix and matrix, the thermal conductivity that macro manifestations is high workability halogen-free flame-retarded heat-conducting matrix material is higher, mechanical property is better, shrinking percentage is lower, resistance toheat is more excellent, and improving the product surface outward appearance, all there is raising in various degree the aspects such as the flame retarding efficiency of fire retardant.This explanation the present invention adopts the high-fluidity nylon that contains side chain nylon 6 as matrix resin, the preparation technology that the characteristic of binding resin matrix and heat conductive filler sets, can effectively solve filler in halogen-free flame-retarded heat-conducting modified nylon process and fire retardant and matrix phase capacitive poor, disperse unequal problem, and this technology has general suitability to the filled-type thermally conductive system.Therefore, can be widely used in by the resulting high-fluidity polyamide base of technology of preparing of the present invention halogen-free flame-retarded heat-conducting matrix material the Electric Plastic part field that the heat radiations such as railway locomotive railway carriage illuminating lamp shade, automobile and civil LED scatterer, household electrical appliances motor housing, laptop, micro-shape projector case, transformer coil frame are had relatively high expectations.
Claims (10)
1. the present invention relates to a kind of high-fluidity polyamide base halogen-free flame-retarded heat-conducting matrix material, it is characterized in that, this matrix material is composed of the following components by weight percentage:
Nylon resin: 5-85;
Heat conductive filler: 10-80;
Halogen-free flame retardants: 1-15;
Oxidation inhibitor: 0.1-0.5;
Coupling agent: 0.1-2.
2. high-fluidity polyamide base halogen-free flame-retarded heat-conducting matrix material according to claim 1 is characterized in that: described nylon resin is a kind of at least containing the high-fluidity nylon composition of branched structure nylon 6.
3. high-fluidity polyamide base halogen-free flame-retarded heat-conducting matrix material according to claim 2, described nylon composite is high-fluidity nylon 6 and nylon 6, nylon 66, nylon 46, nylon 12, nylon 612, the arbitrary combination of nylon 1212 and aromatic nylon.
4. according to the described high-fluidity polyamide base of claim 2 or 3 halogen-free flame-retarded heat-conducting matrix material, it is characterized in that: described high-fluidity nylon 6 resins are 230 in shear temperature
oC, shearing resistance is 500s
-1test condition under, relative viscosity is 1.1-2.8, kinematic viscosity is between 10Pa.s-1000 Pa.s.
5. high-fluidity polyamide base halogen-free flame-retarded heat-conducting matrix material according to claim 1, it is characterized in that: described heat conductive filler component is a kind of or arbitrary combination in magnesium oxide, magnesium nitride, ball-aluminium oxide, class ball-aluminium oxide, aluminium nitride, boron nitride, pitch fibers, halloysite, carbon nanotube, graphite, silicon carbide, boehmite.
6. the high-fluidity polyamide base halogen-free flame-retarded heat-conducting matrix material of stating according to claim 1, it is characterized in that: described halogen-free flame retardants comprises a kind of or arbitrary combination of the agent of phosphorus nitrogen fire-retardant, the agent of alkylphosphonic fire-retardant and inorganic fire-retardant agent, wherein, the agent of phosphorus nitrogen fire-retardant is a kind of or arbitrary combination of trimeric cyanamide-poly-phosphate (MP), trimeric cyanamide-polyphosphoric acid salt (MP) and trimeric cyanamide-focusing phosphoric acid salt; The agent of alkylphosphonic fire-retardant is a kind of or arbitrary combination of alkyl hypophosphite, alkyl metaphosphate or alkyl phosphite; Inorganic fire-retardant agent comprises ammonium polyphosphate (APP), aluminium hydroxide, magnesium hydroxide, expanded polystyrene veneer graphite, sal epsom seven water and molybdenum oxide is a kind of or arbitrary combination.
7. it is characterized in that according to claim 1: the arbitrary combination that described oxidation inhibitor is Hinered phenols antioxidant and phosphite ester kind antioxidant.
8. it is characterized in that according to claim 1: a kind of or arbitrary combination that described coupling agent is silane coupling agent (KH792, KH550, KH560, KH570) or epoxy group(ing) aliphatic polyester.
9. according to the preparation method of the described high-fluidity polyamide base of claim 1-8 halogen-free flame-retarded heat-conducting matrix material, it is characterized in that this preparation method comprises following processing step:
(1) heat conductive filler, coupling agent are joined in high-speed mixer and fully mix;
(2) all mixed things that step (1) obtained join in mixing machine and fully mix with nylon resin, fire retardant, oxidation inhibitor;
(3) all mixed things that step (2) obtained melt extrude by screw extrusion press, through traction, cooling, pelletizing, obtain high-fluidity polyamide base halogen-free flame-retarded heat-conducting matrix material.
10. the preparation method of high-fluidity polyamide base halogen-free flame-retarded heat-conducting matrix material according to claim 9 is characterized in that: the temperature at the barrel rear portion of described forcing machine is that 220 ℃-250 ℃, the temperature at barrel middle part are that 250 ℃-280 ℃, the temperature of barrel front portion are that 270 ℃-280 ℃, nozzle temperature are 275 ℃-280 ℃; Screw speed is 180-350r/min; Rate of feeding is 10-20r/min.
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| CN112662168A (en) * | 2020-12-04 | 2021-04-16 | 株洲时代工程塑料实业有限公司 | Antibacterial mildew preventive, halogen-free flame-retardant antibacterial mildew-proof nylon composite material, and preparation method and application thereof |
| CN112662168B (en) * | 2020-12-04 | 2022-09-09 | 株洲时代工程塑料实业有限公司 | Antibacterial mildew preventive, halogen-free flame-retardant antibacterial mildew-proof nylon composite material, and preparation method and application thereof |
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