CN102040830A - Polyamide composition and preparation method thereof - Google Patents
Polyamide composition and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polyamide composition and a preparation method thereof, and the polyamide composition comprises the following components by weight percent: 30%-70% of first polyamide resin, 5%-50% of second polyamide resin, 7%-17% of flame retardant, 1%-3% of flame-retardant synergist, 5%-15% of inorganic reinforcing material, 5%-30% of inorganic filler, 0-2% of antioxidant and 0-2% of lubricant, wherein the intrinsic viscosity of the second polyamide resin is lower than that of the first polyamide resin. The first polyamide with high viscosity is utilized for ensuring that the material has certain toughness and rigidity, the material is easier to be reset to the original state after external force is eliminated, and the deformation is further smaller after the material is subject to high temperature; and the second polyamide with the lower viscosity is simultaneously utilized for providing sufficient fluidity, thereby reducing the generation of internal stress during the molding process and ensuring that the material has low deformation amount after molding. The obtained material has smaller warp during high-temperature treatment during and after molding, and can meet the strict requirement of precision electronic devices on warp deformation.
Description
Technical field
The present invention relates to the engineering plastics technical field, relate to a kind of daiamid composition and preparation method.
Background technology
Polymeric amide, is widely used in the machinery etc. at trolley part, electric, electronic unit owing to have excellent forming process.Mainly based on nylon 6 and nylon 66, still along with science and technology development, surface mounting technology is used more and more widely in early days, and the thermotolerance of nylon 6 and nylon 66 just demonstrates deficiency, and therefore needing more, the polymeric amide of high heat resistance satisfies service requirements.
Kai Fa heat-resisting nylon is PA46 the earliest, but there is the problem that has a big risk in water-intake rate height, the use in it; Release one after another PA6T and PA9T heat-resistant polyamide of market thus, and I have taken charge of independent research and have synthesized a kind of novel have high heat resistance and low water absorbable polyamide resin PA10T(patent CN 101456949A), can obtain the limiting viscosity scope at 0.5-3.0dl/g according to service requirements, melting range is at 270-325
oC is for follow-up study on the modification has been established solid basis.
And the polymeric amide that in electric, uses, require it to have flame retardant resistance, usually to reach V-0 fire-retardant by adding halogen compounds for polymeric amide, but halogenous polyamide plastics can discharge the material that contains halogen in the burning disposal process, seriously polluted to human body infringement and environment.Along with the more and more higher environmental requirement of cry in this year, the fire-retardant non-halogen inexorable trend that becomes Future Development of polymeric amide.EMS discloses a kind of halogen-free flameproof in patent WO2004/090036, the polymeric amide of mechanical property improvement simultaneously is used for electronics, electrical industry assembly; Dupont also discloses the fire-retardant Amilan polyamide resin composition of a kind of hypophosphite in patent WO2005/033192, need to be used to the electric component and the electronic unit of electrical insulating property.But all do not relate to product warpage properties problem.
Mitsui discloses a kind of mobile excellent in patent WO2008/062755, and the bromine that the formed body amount of warpage is little is a Flameproof polyamide; Kuraray also discloses a kind of mechanical property excellence in relevant report, the bromine that the moulding amount of warpage is little is the Flameproof polyamide system, but does not see the report of the low warpage patent of polymeric amide halogen-free flameproof so far.
In recent years, because the preparation of electronic unit is more and more accurate, the daiamid composition that require to use has still less warpage to satisfy this demand in moulded products, further require not only when moulding, and carry out having less warpage properties in the pyroprocessing after moulding.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of daiamid composition that not only carries out having in the pyroprocessing less warpage when moulding but also after moulding is provided.
Another object of the present invention is to provide the preparation method of above-mentioned daiamid composition.
To achieve these goals, the present invention adopts following technical scheme:
A kind of daiamid composition, form by the component of following weight percentage:
The first polyamide resin 30%-70%
The second polyamide resin 5%-50%
Fire retardant 7%-17%
Fire retarding synergist 1%-3%
Inorganic reinforcement 5%-15%
Mineral filler 5%-30%
Oxidation inhibitor 0-2%
Lubricant 0-2%;
The described first polyamide resin limiting viscosity is equal to or greater than 1.5dl/g, and fusing point is 295-325
oC;
The described second polyamide resin limiting viscosity is lower than first polyamide resin, and fusing point is 270-290
oC.
In above-mentioned daiamid composition, the repeating unit of described first polyamide resin or second polyamide resin is selected from terephthalic acid, m-phthalic acid, 2-methyl terephthalic acid, 2,5-dichloroterephthalicacid acid, 2,6-is dioctyl phthalate, 1 how, 4-is dioctyl phthalate, 4 how, 4 '-biphenyl dicarboxylic acid or 2,2 '-biphenyl dicarboxylic acid, 1,6-hexanediamine, 1,10-decamethylene diamine, 1,9-nonamethylene diamine, diethylenetriamine, triethylene tetramine, tetraene five amine, polyethylene polyamine or isophthaloyl-1, the 6-hexanediamine.In above-mentioned daiamid composition, described fire retardant is one or both mixing in phosphinates or the bisphosphinic acid salt.
In above-mentioned daiamid composition, described fire retarding synergist is zinc borate, zinc oxide, zeolite or glass fibre.
In above-mentioned daiamid composition, described antioxidant is selected from one or more mixing in phenol antioxidant, thioether class antioxidant and the phosphite antioxidant.
In above-mentioned daiamid composition, described inorganic reinforcement is one or more mixing in glass fibre, wollastonite fibre, steel fiber, the boric acid fibre.
In above-mentioned daiamid composition, described mineral filler is one or more mixing in glass flake, mica, talcum powder, graphite, kaolin, glass microballon, titanium dioxide, silicon-dioxide, aluminum oxide, boron nitride, aluminium nitride, barium sulfate, lime carbonate, the calcium sulfate.
In above-mentioned daiamid composition, described lubricant is one or more mixing in low-molecular-weight polypropylene, polyethylene wax, montanic acid sodium salt, the hyperbranched polymer.
The preparation method who states daiamid composition comprises the steps:
(1) premix is carried out in lubricant, oxidation inhibitor, fire retarding synergist and mineral filler earlier in high mixer, obtain Preblend 1;
(2) premix in high mixer with first polyamide resin and second polyamide resin obtains Preblend 2;
(3) Preblend 1 and the Preblend 2 that obtains is added twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed a mouthful adding twin screw extruder from side in proportion with weigher respectively, extruding pelletization obtains the daiamid composition pellet.
Compared with prior art, the present invention has following beneficial effect:
Sharpest edges of the present invention are to utilize full-bodied first polymeric amide to guarantee that material has certain toughness and rigidity, and material easier original state that is returned to after external force is eliminated is crossed the high temperature after strain then and diminished like this; Utilize the second lower polymeric amide of viscosity that enough flowabilities are provided simultaneously, reduce the generation of internal stress in the moulding process, guarantee after moulding, to have low deflection.Thereby the material that obtains not only has less buckling deformation amount when moulding, and still has less buckling deformation amount in the pyroprocessing after moulding, can satisfy the strict demand of precise electronic device to buckling deformation.
Embodiment
The invention will be further described below in conjunction with embodiment, and described ratio is weight and forms.
The moulded products warpage is estimated:
With the daiamid composition granulation material that will estimate 120
oBehind dry 4 hours of the C, use to have the injection moulding machine (HAITIAN HTF86/TJ) of plate-like metal die with 310
oThe barrel temperature of C and 110
oThe die temperature of C is with the pellet moulding, and obtaining diameter is that 64mm and thickness are the disk samples of 0.5mm.Then, the sample that obtains is placed on the flat board, the periphery of dish is got plane for referencial use, and will get and make door section, use micrometer to measure height from reference plane to the door section, check displacement away from the part of flat board.The numerical value that obtains promptly is the buckling deformation amount of moulding rear forming product.
Then, the sample of having measured buckling deformation is put into reflow machine handle, the reflow machine peak temperature is set to 260
oC, the total elapsed-time standards of Reflow Soldering is about 6min.After the processing, take out sample, adopt method same as described above to detect the buckling deformation amount, the numerical value of acquisition promptly is the amount of warpage after the thermal treatment.
The warpage test adopts the Dongguan TESA of three precision instrument company limiteds digital display height calipers to measure.
Embodiment 1
Daiamid composition, its each component percentages is first polyamide resin (poly-decamethylene terephthaloyl amine PA10T, 310 ℃ of fusing points, limiting viscosity is 1.9dl/g) 35%, second polyamide resin (decamethylene terephthaloyl amine and hexa-methylene adipamide copolymer p A10T/66,285 ℃ of fusing points, limiting viscosity are 0.8 dl/g)) 15%, rounded section glass fibre 25%, mica powder 8%, phosphinates fire retardant 15%, zinc borate 1%, phenolic antioxidant 0.3%, polyethylene wax 0.7%.
Premix is carried out in lubricant, oxidation inhibitor, fire retarding synergist and mineral filler earlier in high mixer, obtain Preblend 1; The premix in high mixer with first polyamide resin and second polyamide resin obtains Preblend 2 again; At last Preblend 1 and the Preblend 2 that obtains is added twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed a mouthful adding twin screw extruder from side in proportion with weigher respectively, extruding pelletization obtains the daiamid composition pellet.
The parameters test result of the daiamid composition that this embodiment provided sees Table 1.
Embodiment 2
Daiamid composition, its each component percentages is first polyamide resin (hexa-methylene terephthaloyl amine and an isophthaloyl-1,6-hexanediamine PA6T/6I, 320 ℃ of fusing points, limiting viscosity is 2.0dl/g)) 25%, second polyamide resin (hexa-methylene terephthaloyl amine and hexa-methylene adipamide copolymer p A6T/66,280 ℃ of fusing points, limiting viscosity are 0.9dl/g)) 25%, rounded section glass fibre 25%, mica powder 8%, phosphinates fire retardant 15%, zinc borate 1%, phenolic antioxidant 0.3%, polyethylene wax 0.7%.
Premix is carried out in lubricant, oxidation inhibitor, fire retarding synergist and mineral filler earlier in high mixer, obtain Preblend 1; The premix in high mixer with first polyamide resin and second polyamide resin obtains Preblend 2 again; At last Preblend 1 and the Preblend 2 that obtains is added twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed a mouthful adding twin screw extruder from side in proportion with weigher respectively, extruding pelletization obtains the daiamid composition pellet.
The parameters test result of the daiamid composition that this embodiment provided sees Table 1.
Embodiment 3
Daiamid composition, its each component percentages is first polyamide resin (poly-decamethylene terephthaloyl amine PA10T, 310 ℃ of fusing points, limiting viscosity is 2.1dl/g)) 15%, second polyamide resin (decamethylene terephthaloyl amine and hexa-methylene adipamide copolymer p A10T/66,285 ℃ of fusing points, limiting viscosity are 0.9dl/g)) 35%, rounded section glass fibre 25%, mica powder 8%, phosphinates fire retardant 15%, zinc borate 1%, phenolic antioxidant 0.3%, polyethylene wax 0.7%.
Premix is carried out in lubricant, oxidation inhibitor, fire retarding synergist and mineral filler earlier in high mixer, obtain Preblend 1; The premix in high mixer with first polyamide resin and second polyamide resin obtains Preblend 2 again; At last Preblend 1 and the Preblend 2 that obtains is added twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed a mouthful adding twin screw extruder from side in proportion with weigher respectively, extruding pelletization obtains the daiamid composition pellet.
The parameters test result of the daiamid composition that this embodiment provided sees Table 1.
Embodiment 4
Daiamid composition, its each component percentages is first polyamide resin (poly-decamethylene terephthaloyl amine PA10T, 310 ℃ of fusing points, limiting viscosity is 1.9dl/g)) 20%, second polyamide resin (hexa-methylene terephthaloyl amine and m-phthalic acid-1,6-hexanediamine copolymer p A6T/6I/66,290 ℃ of fusing points, limiting viscosity are 1.0dl/g)) 30%, rounded section glass fibre 25%, mica powder 8%, phosphinates fire retardant 15%, zinc borate 1%, phenolic antioxidant 0.3%, polyethylene wax 0.7%.
Premix is carried out in lubricant, oxidation inhibitor, fire retarding synergist and mineral filler earlier in high mixer, obtain Preblend 1; The premix in high mixer with first polyamide resin and second polyamide resin obtains Preblend 2 again; At last Preblend 1 and the Preblend 2 that obtains is added twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed a mouthful adding twin screw extruder from side in proportion with weigher respectively, extruding pelletization obtains the daiamid composition pellet.
The parameters test result of the daiamid composition that this embodiment provided sees Table 1.
Embodiment 5
Daiamid composition, its each component percentages is first polyamide resin (poly-decamethylene terephthaloyl amine PA10T, 310 ℃ of fusing points, limiting viscosity is 2.6dl/g)) 30%, second polyamide resin (decamethylene terephthaloyl amine and hexa-methylene adipamide copolymer p A10T/66,285 ℃ of fusing points, limiting viscosity are 0.7dl/g)) 20%, rounded section glass fibre 25%, mica powder 8%, phosphinates fire retardant 15%, zinc borate 1%, phenolic antioxidant 0.3%, polyethylene wax 0.7%.
Premix is carried out in lubricant, oxidation inhibitor, fire retarding synergist and mineral filler earlier in high mixer, obtain Preblend 1; The premix in high mixer with first polyamide resin and second polyamide resin obtains Preblend 2 again; At last Preblend 1 and the Preblend 2 that obtains is added twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed a mouthful adding twin screw extruder from side in proportion with weigher respectively, extruding pelletization obtains the daiamid composition pellet.
The parameters test result of the daiamid composition that this Comparative Examples provided sees Table 1.
Comparative Examples 1
Daiamid composition, its each component percentages is first polyamide resin (poly-decamethylene terephthaloyl amine PA10T, 310 ℃ of fusing points, limiting viscosity is 1.9dl/g)) 30%, second polyamide resin (decamethylene terephthaloyl amine and hexa-methylene adipamide copolymer p A10T/66,285 ℃ of fusing points, limiting viscosity are 0.8dl/g)) 20%, ellipse or square-section, aspect ratio be 4-6 glass fibre 25%, mica powder 8%, phosphinates fire retardant 15%, zinc borate 1%, phenolic antioxidant 0.3%, polyethylene wax 0.7%.
Premix is carried out in lubricant, oxidation inhibitor, fire retarding synergist and mineral filler earlier in high mixer, obtain Preblend 1; The premix in high mixer with first polyamide resin and second polyamide resin obtains Preblend 2 again; At last Preblend 1 and the Preblend 2 that obtains is added twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed a mouthful adding twin screw extruder from side in proportion with weigher respectively, extruding pelletization obtains the daiamid composition pellet.
The parameters test result of the daiamid composition that this Comparative Examples provided sees Table 1.
Comparative Examples 2
Daiamid composition, its each component percentages is first polyamide resin (poly-decamethylene terephthaloyl amine PA10T, 310 ℃ of fusing points, limiting viscosity is 1.9dl/g)) 20%, second polyamide resin (decamethylene terephthaloyl amine and hexa-methylene adipamide copolymer p A10T/66,285 ℃ of fusing points, limiting viscosity are 0.8dl/g)) 30%, ellipse or square-section, aspect ratio be 4-6 glass fibre 25%, mica powder 8%, phosphinates fire retardant 15%, zinc borate 1%, phenolic antioxidant 0.3%, polyethylene wax 0.7%.
Premix is carried out in lubricant, oxidation inhibitor, fire retarding synergist and mineral filler earlier in high mixer, obtain Preblend 1; The premix in high mixer with first polyamide resin and second polyamide resin obtains Preblend 2 again; At last Preblend 1 and the Preblend 2 that obtains is added twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed a mouthful adding twin screw extruder from side in proportion with weigher respectively, extruding pelletization obtains the daiamid composition pellet.
The parameters test result of the daiamid composition that this Comparative Examples provided sees Table 1.
Comparative Examples 3
Daiamid composition, its each component percentages is first polyamide resin (poly-decamethylene terephthaloyl amine PA10T, 310 ℃ of fusing points, limiting viscosity are 2.0dl/g)) 50%, rounded section glass fibre 25%, mica powder 8%, phosphinates fire retardant 15%, zinc borate 1%, phenolic antioxidant 0.3%, polyethylene wax 0.7%.
Premix is carried out in lubricant, oxidation inhibitor, fire retarding synergist and mineral filler earlier in high mixer, obtain Preblend 1; The Preblend 1 and first polyamide resin that obtain are added twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed a mouthful adding twin screw extruder from side in proportion with weigher respectively, extruding pelletization obtains the daiamid composition pellet.
The parameters test result of the daiamid composition that this Comparative Examples provided sees Table 1.
Comparative Examples 4
Daiamid composition, its each component percentages is second polyamide resin (decamethylene terephthaloyl amine and hexa-methylene adipamide copolymer p A10T/66,285 ℃ of fusing points, limiting viscosity are 0.8dl/g)) 50%, rounded section glass fibre 25%, mica powder 8%, phosphinates fire retardant 15%, zinc borate 1%, phenolic antioxidant 0.3%, polyethylene wax 0.7%.
Premix is carried out in lubricant, oxidation inhibitor, fire retarding synergist and mineral filler earlier in high mixer, obtain Preblend 1; The Preblend 1 and second polyamide resin that obtain are added twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed a mouthful adding twin screw extruder from side in proportion with weigher respectively, extruding pelletization obtains the daiamid composition pellet.
The parameters test result of the daiamid composition that this Comparative Examples provided sees Table 1.
Each embodiment of table 1 and Comparative Examples parameter testing result
By table 1 result as can be seen, by the ratio of two kinds of polymeric amide of suitable adjustment, the daiamid composition moulding product that obtain not only have less buckling deformation amount when moulding, and still have less buckling deformation amount in the pyroprocessing after moulding.
Claims (9)
1. daiamid composition, form by the component of following weight percentage:
The first polyamide resin 30%-70%
The second polyamide resin 5%-50%
Fire retardant 7%-17%
Fire retarding synergist 1%-3%
Inorganic reinforcement 5%-15%
Mineral filler 5%-30%
Oxidation inhibitor 0-2%
Lubricant 0-2%;
The described first polyamide resin limiting viscosity is equal to or greater than 1.5dl/g, and fusing point is 295-325
oC;
The described second polyamide resin limiting viscosity is lower than first polyamide resin, and fusing point is 270-290
oC.
2. daiamid composition as claimed in claim 1, the repeating unit that it is characterized in that described first polyamide resin or second polyamide resin is selected from terephthalic acid, m-phthalic acid, 2-methyl terephthalic acid, 2,5-dichloroterephthalicacid acid, 2,6-is dioctyl phthalate, 1 how, 4-is dioctyl phthalate, 4 how, 4 '-biphenyl dicarboxylic acid or 2,2 '-biphenyl dicarboxylic acid, 1,6-hexanediamine, 1,10-decamethylene diamine, 1,9-nonamethylene diamine, diethylenetriamine, triethylene tetramine, tetraene five amine, polyethylene polyamine or isophthaloyl-1, the 6-hexanediamine.
3. daiamid composition as claimed in claim 1 is characterized in that described fire retardant is one or both mixing in phosphinates or the bisphosphinic acid salt.
4. daiamid composition as claimed in claim 1 is characterized in that described fire retarding synergist is zinc borate, zinc oxide, zeolite or glass fibre.
5. daiamid composition as claimed in claim 1 is characterized in that described antioxidant is selected from one or more mixing in phenol antioxidant, thioether class antioxidant and the phosphite antioxidant.
6. daiamid composition as claimed in claim 1 is characterized in that described inorganic reinforcement is one or more mixing in glass fibre, wollastonite fibre, steel fiber, the boric acid fibre.
7. daiamid composition as claimed in claim 1 is characterized in that described mineral filler is one or more mixing in glass flake, mica, talcum powder, graphite, kaolin, glass microballon, titanium dioxide, silicon-dioxide, aluminum oxide, boron nitride, aluminium nitride, barium sulfate, lime carbonate, the calcium sulfate.
8. daiamid composition as claimed in claim 1 is characterized in that described lubricant is one or more mixing in low-molecular-weight polypropylene, polyethylene wax, montanic acid sodium salt, the hyperbranched polymer.
9. the preparation method of the described daiamid composition of claim 1 is characterized in that comprising the steps:
(1) premix is carried out in lubricant, oxidation inhibitor, fire retarding synergist and mineral filler earlier in high mixer, obtain Preblend 1;
(2) premix in high mixer with first polyamide resin and second polyamide resin obtains Preblend 2;
(3) Preblend 1 and the Preblend 2 that obtains is added twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed a mouthful adding twin screw extruder from side in proportion with weigher respectively, extruding pelletization obtains the daiamid composition pellet.
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