CN102040830B - Polyamide composition and preparation method thereof - Google Patents
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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 engineering plastics technical field, relate to a kind of daiamid composition and preparation method.
Background technology
Polymeric amide, owing to having excellent forming process, at trolley part, electric, electronic unit, is widely used in machinery etc.Mainly take nylon 6 and nylon 66 in early days as main, but along with scientific and technical development, surface mounting technology application is more and more extensive, and the thermotolerance of nylon 6 and nylon 66 just demonstrates deficiency, therefore needs the more polymeric amide of high heat resistance to meet service requirements.
The heat-resisting nylon of exploitation is PA46 the earliest, but it exists, water-intake rate is high, the large problem of use risk; 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), according to requirements can obtain limiting viscosity scope at 0.5-3.0dl/g, melting range is at 270-325
oc, for follow-up study on the modification has been established solid basis.
And at the polymeric amide of electric middle use, require it to there is flame retardant resistance, conventionally polymeric amide is fire-retardant by adding halogen compounds to reach V-0, but the polyamide plastics of Halogen can discharge the material that contains halogen in 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, and the polymeric amide that mechanical property is improved simultaneously, for electronics, electrical industry assembly; Dupont also discloses the fire-retardant Amilan polyamide resin composition of a kind of hypophosphite in patent WO2005/033192, for needing electric component and the electronic unit of electrical insulating property.But all do not relate to product warpage properties problem.
It is excellent that Mitsui discloses a kind of mobility in patent WO2008/062755, and the bromine that formed body amount of warpage is little is Flameproof polyamide; It is excellent that Kuraray also discloses a kind of mechanical property in relevant report, and the bromine that moulding amount of warpage is little is Flameproof polyamide system, the report of the low warpage patent of polyamide halogen-free flame retardant that still so far there are no.
In recent years, because the preparation of electronic unit is more and more accurate, the daiamid composition require using has warpage still less to meet this demand in moulded products, further requires not only when moulding, and after moulding, carries out in pyroprocessing, having less warpage properties.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of daiamid composition that not only carries out having in 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 daiamid composition, is comprised of 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%;
Described the first polyamide resin limiting viscosity is equal to or greater than 1.5dl/g, and fusing point is 295-325
oc;
Described the second polyamide resin limiting viscosity is lower than the first polyamide resin, and fusing point is 270-290
oc.
In above-mentioned daiamid composition, the repeating unit of described the first polyamide resin or the 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-1,6-hexanediamine.In above-mentioned daiamid composition, described fire retardant is one or both mixing in phosphinates or 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 phosphite antioxidant.
In above-mentioned daiamid composition, described inorganic reinforcement is one or more mixing in glass fibre, wollastonite fibre, steel fiber, 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, calcium carbonate, 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, hyperbranched polymer.
The preparation method who states daiamid composition comprises the steps:
(1) lubricant, oxidation inhibitor, fire retarding synergist and mineral filler are first carried out in high mixer to premix, obtained Preblend 1;
(2) premix in high mixer by the first polyamide resin and the second polyamide resin, obtains Preblend 2;
(3) Preblend obtaining 1 and Preblend 2 are added to twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed mouth from side in proportion with weigher respectively and are added twin screw extruder, extruding pelletization, obtains 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 the first polymeric amide to guarantee that material has certain toughness and rigidity, and material is more easily returned to original state after external force is eliminated like this, then cross high temperature after strain and diminish; Utilize the second polymeric amide that viscosity is lower that enough mobility are provided simultaneously, reduce the generation of internal stress in moulding process, guarantee after moulding, to there is low deflection.Thereby the material obtaining not only has less buckling deformation amount when moulding, and in the pyroprocessing after moulding, still there is less buckling deformation amount, can meet the strict demand of precise electronic device to buckling deformation.
Embodiment
Below in conjunction with embodiment, the invention will be further described, and described ratio is weight and forms.
Moulded products warpage is evaluated:
By the daiamid composition granulation material that will evaluate 120
oc is dry after 4 hours, uses the injection moulding machine (HAITIAN HTF86/TJ) with plate-like metal die with 310
othe barrel temperature of C and 110
othe die temperature of C is by pellet moulding, and obtaining diameter is the disk samples that 64mm and thickness are 0.5mm.Then, the sample of acquisition is placed on to flat board upper, the periphery of dish is got to plane for referencial use, and make door section by getting away from dull and stereotyped part, use micrometer to measure the height from reference plane to door section, check displacement.The numerical value obtaining be the buckling deformation amount of moulding rear forming product.
Then, the sample of having measured buckling deformation is put into reflow machine and process, reflow machine peak temperature is set to 260
oc, the total elapsed-time standards of Reflow Soldering is about 6min.After processing, take out sample, adopt method same as described above to detect buckling deformation amount, the numerical value of acquisition be the amount of warpage after thermal treatment.
Warpage test adopts the Dongguan San Ben precision instrument TESA of company limited digital display height calipers to measure.
Embodiment 1
Daiamid composition, its each component percentages is the first polyamide resin (poly-decamethylene terephthaloyl amine PA10T, 310 ℃ of fusing points, limiting viscosity is 1.9dl/g) the 35%, second polyamide resin (decamethylene terephthaloyl amine and hexa-methylene adipamide copolymer p A10T/66,285 ℃ of fusing points, limiting viscosity is 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%.
Lubricant, oxidation inhibitor, fire retarding synergist and mineral filler are first carried out in high mixer to premix, obtained Preblend 1; The premix in high mixer by the first polyamide resin and the second polyamide resin, obtains Preblend 2 again; Finally the Preblend obtaining 1 and Preblend 2 are added to twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed mouth from side in proportion with weigher respectively and are added twin screw extruder, extruding pelletization, obtains daiamid composition pellet.
The parameters test result of the daiamid composition that this embodiment provides is in Table 1.
Embodiment 2
Daiamid composition, its each component percentages is the first polyamide resin (hexa-methylene terephthaloyl amine and isophthaloyl-1,6-hexanediamine PA6T/6I, 320 ℃ of fusing points, limiting viscosity is 2.0dl/g)) the 25%, second polyamide resin (hexa-methylene terephthaloyl amine and hexa-methylene adipamide copolymer p A6T/66,280 ℃ of fusing points, limiting viscosity is 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%.
Lubricant, oxidation inhibitor, fire retarding synergist and mineral filler are first carried out in high mixer to premix, obtained Preblend 1; The premix in high mixer by the first polyamide resin and the second polyamide resin, obtains Preblend 2 again; Finally the Preblend obtaining 1 and Preblend 2 are added to twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed mouth from side in proportion with weigher respectively and are added twin screw extruder, extruding pelletization, obtains daiamid composition pellet.
The parameters test result of the daiamid composition that this embodiment provides is in Table 1.
Embodiment 3
Daiamid composition, its each component percentages is the first polyamide resin (poly-decamethylene terephthaloyl amine PA10T, 310 ℃ of fusing points, limiting viscosity is 2.1dl/g)) the 15%, second polyamide resin (decamethylene terephthaloyl amine and hexa-methylene adipamide copolymer p A10T/66,285 ℃ of fusing points, limiting viscosity is 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%.
Lubricant, oxidation inhibitor, fire retarding synergist and mineral filler are first carried out in high mixer to premix, obtained Preblend 1; The premix in high mixer by the first polyamide resin and the second polyamide resin, obtains Preblend 2 again; Finally the Preblend obtaining 1 and Preblend 2 are added to twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed mouth from side in proportion with weigher respectively and are added twin screw extruder, extruding pelletization, obtains daiamid composition pellet.
The parameters test result of the daiamid composition that this embodiment provides is in Table 1.
Embodiment 4
Daiamid composition, its each component percentages is the first polyamide resin (poly-decamethylene terephthaloyl amine PA10T, 310 ℃ of fusing points, limiting viscosity is 1.9dl/g)) the 20%, second polyamide resin (hexa-methylene terephthaloyl amine and m-phthalic acid-1,6-hexamethylene diamine copolymer PA6T/6I/66,290 ℃ of fusing points, limiting viscosity is 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%.
Lubricant, oxidation inhibitor, fire retarding synergist and mineral filler are first carried out in high mixer to premix, obtained Preblend 1; The premix in high mixer by the first polyamide resin and the second polyamide resin, obtains Preblend 2 again; Finally the Preblend obtaining 1 and Preblend 2 are added to twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed mouth from side in proportion with weigher respectively and are added twin screw extruder, extruding pelletization, obtains daiamid composition pellet.
The parameters test result of the daiamid composition that this embodiment provides is in Table 1.
Embodiment 5
Daiamid composition, its each component percentages is the first polyamide resin (poly-decamethylene terephthaloyl amine PA10T, 310 ℃ of fusing points, limiting viscosity is 2.6dl/g)) the 30%, second polyamide resin (decamethylene terephthaloyl amine and hexa-methylene adipamide copolymer p A10T/66,285 ℃ of fusing points, limiting viscosity is 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%.
Lubricant, oxidation inhibitor, fire retarding synergist and mineral filler are first carried out in high mixer to premix, obtained Preblend 1; The premix in high mixer by the first polyamide resin and the second polyamide resin, obtains Preblend 2 again; Finally the Preblend obtaining 1 and Preblend 2 are added to twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed mouth from side in proportion with weigher respectively and are added twin screw extruder, extruding pelletization, obtains daiamid composition pellet.
The parameters test result of the daiamid composition that this comparative example provides is in Table 1.
Comparative example 1
Daiamid composition, its each component percentages is the first polyamide resin (poly-decamethylene terephthaloyl amine PA10T, 310 ℃ of fusing points, limiting viscosity is 1.9dl/g)) the 30%, second polyamide resin (decamethylene terephthaloyl amine and hexa-methylene adipamide copolymer p A10T/66,285 ℃ of fusing points, limiting viscosity is 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%.
Lubricant, oxidation inhibitor, fire retarding synergist and mineral filler are first carried out in high mixer to premix, obtained Preblend 1; The premix in high mixer by the first polyamide resin and the second polyamide resin, obtains Preblend 2 again; Finally the Preblend obtaining 1 and Preblend 2 are added to twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed mouth from side in proportion with weigher respectively and are added twin screw extruder, extruding pelletization, obtains daiamid composition pellet.
The parameters test result of the daiamid composition that this comparative example provides is in Table 1.
Comparative example 2
Daiamid composition, its each component percentages is the first polyamide resin (poly-decamethylene terephthaloyl amine PA10T, 310 ℃ of fusing points, limiting viscosity is 1.9dl/g)) the 20%, second polyamide resin (decamethylene terephthaloyl amine and hexa-methylene adipamide copolymer p A10T/66,285 ℃ of fusing points, limiting viscosity is 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%.
Lubricant, oxidation inhibitor, fire retarding synergist and mineral filler are first carried out in high mixer to premix, obtained Preblend 1; The premix in high mixer by the first polyamide resin and the second polyamide resin, obtains Preblend 2 again; Finally the Preblend obtaining 1 and Preblend 2 are added to twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed mouth from side in proportion with weigher respectively and are added twin screw extruder, extruding pelletization, obtains daiamid composition pellet.
The parameters test result of the daiamid composition that this comparative example provides is in Table 1.
Comparative example 3
Daiamid composition, its each component percentages is the first polyamide resin (poly-decamethylene terephthaloyl amine PA10T, 310 ℃ of fusing points, limiting viscosity is 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%.
Lubricant, oxidation inhibitor, fire retarding synergist and mineral filler are first carried out in high mixer to premix, obtained Preblend 1; The Preblend obtaining 1 and the first polyamide resin are added to twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed mouth from side in proportion with weigher respectively and are added twin screw extruder, extruding pelletization, obtains daiamid composition pellet.
The parameters test result of the daiamid composition that this comparative example provides is in Table 1.
Comparative example 4
Daiamid composition, its each component percentages is the second polyamide resin (decamethylene terephthaloyl amine and hexa-methylene adipamide copolymer p A10T/66,285 ℃ of fusing points, limiting viscosity is 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%.
Lubricant, oxidation inhibitor, fire retarding synergist and mineral filler are first carried out in high mixer to premix, obtained Preblend 1; The Preblend obtaining 1 and the second polyamide resin are added to twin screw extruder from main spout in proportion by weigher respectively, inorganic reinforcement and fire retardant are fed mouth from side in proportion with weigher respectively and are added twin screw extruder, extruding pelletization, obtains daiamid composition pellet.
The parameters test result of the daiamid composition that this comparative example provides is in Table 1.
Each embodiment of table 1 and comparative example parameter testing result
By table 1 result, can be found out, by the ratio of two kinds of polymeric amide of suitable adjustment, the daiamid composition products formed obtaining not only has less buckling deformation amount when moulding, and in the pyroprocessing after moulding, still has less buckling deformation amount.
Claims (1)
1. a daiamid composition, each component weight percentage is selected from following combination:
(1) poly-decamethylene terephthaloyl amine PA10T 35%, 285 ℃ of fusing points, the limiting viscosity that 310 ℃ of fusing points, limiting viscosity are 1.9dl/g is the decamethylene terephthaloyl amine of 0.8 dl/g and hexa-methylene adipamide copolymer p A10T/66 15%, rounded section glass fibre 25%, mica powder 8%, phosphinates fire retardant 15%, zinc borate 1%, phenolic antioxidant 0.3%, polyethylene wax 0.7%;
(2) 320 ℃ of fusing points, limiting viscosity are 2.0dl/g hexa-methylene terephthaloyl amine and isophthaloyl-1, the hexa-methylene terephthaloyl amine that 6-hexanediamine PA6T/6I 25%, 280 ℃ of fusing points, limiting viscosity are 0.9dl/g and hexa-methylene adipamide copolymer p A6T/66 25%, rounded section glass fibre 25%, mica powder 8%, phosphinates fire retardant 15%, zinc borate 1%, phenolic antioxidant 0.3%, polyethylene wax 0.7%;
(3) the decamethylene terephthaloyl amine that poly-decamethylene terephthaloyl amine PA10T 15%, 285 ℃ of fusing points, the limiting viscosity that 310 ℃ of fusing points, limiting viscosity are 2.1dl/g is 0.9dl/g and hexa-methylene adipamide copolymer p A10T/66 35%, rounded section glass fibre 25%, mica powder 8%, phosphinates fire retardant 15%, zinc borate 1%, phenolic antioxidant 0.3%, polyethylene wax 0.7%;
(4) hexa-methylene terephthaloyl amine and m-phthalic acid-1 that poly-decamethylene terephthaloyl amine PA10T 20%, 290 ℃ of fusing points, the limiting viscosity that 310 ℃ of fusing points, limiting viscosity are 1.9dl/g is 1.0dl/g, 6-hexamethylene diamine copolymer PA6T/6I/66 30%, rounded section glass fibre 25%, mica powder 8%, phosphinates fire retardant 15%, zinc borate 1%, phenolic antioxidant 0.3%, polyethylene wax 0.7%;
(5) the decamethylene terephthaloyl amine that poly-decamethylene terephthaloyl amine PA10T 30%, 285 ℃ of fusing points, the limiting viscosity that 310 ℃ of fusing points, limiting viscosity are 2.6dl/g is 0.7dl/g and hexa-methylene adipamide copolymer p A10T/66 20%, rounded section glass fibre 25%, mica powder 8%, phosphinates fire retardant 15%, zinc borate 1%, phenolic antioxidant 0.3%, polyethylene wax 0.7%.
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| CN102732014A (en) * | 2012-06-15 | 2012-10-17 | 苏州宇度医疗器械有限责任公司 | Flame-retardant polyamide high-molecular material filled with calcium sulfate whiskers |
| CN103627165B (en) * | 2012-08-29 | 2016-07-06 | 汉达精密电子(昆山)有限公司 | High-viscosity glass fibre-reinforced polyamide resin and preparation method |
| CN103073881B (en) * | 2012-09-17 | 2014-12-24 | 天津金发新材料有限公司 | Nylon composition, preparation method and applications thereof |
| CN103254424A (en) * | 2013-05-20 | 2013-08-21 | 金发科技股份有限公司 | Polyamide resin and polyamide composition composed thereof |
| CN103333335A (en) * | 2013-06-21 | 2013-10-02 | 金发科技股份有限公司 | High-fluidity PA10T polyamide resin and polyamide composition comprising same |
| CN103342811A (en) * | 2013-07-12 | 2013-10-09 | 金发科技股份有限公司 | High-flowability PA10T polyamide prepolymer and polyamide composition comprising same |
| CN103642036A (en) * | 2013-11-12 | 2014-03-19 | 金发科技股份有限公司 | Polyamide resin and polyamide composition composed of same |
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| CN106433116B (en) * | 2016-09-27 | 2019-06-14 | 广东中塑新材料有限公司 | High temperature resistant copolyamide 6T composition and preparation method thereof |
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| CN106633858B (en) * | 2017-01-10 | 2019-01-04 | 江门市德众泰工程塑胶科技有限公司 | A kind of polyamide resin composite material and its preparation method and application |
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| CN111621146B (en) * | 2020-06-30 | 2023-05-12 | 重庆科聚孚工程塑料有限责任公司 | Low-water-absorption polyamide material and preparation method thereof |
| CN111675898B (en) * | 2020-06-30 | 2023-05-12 | 重庆科聚孚工程塑料有限责任公司 | Low-water-absorption toughened polyamide material and preparation method thereof |
| CN116554676B (en) * | 2023-04-28 | 2024-10-29 | 珠海万通特种工程塑料有限公司 | Polyamide composition and preparation method and application thereof |
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| DE19983137B4 (en) * | 1998-04-24 | 2009-04-02 | Chisso Corp. | Flame retardant polyolefin composition |
| JP2003119378A (en) * | 2000-09-12 | 2003-04-23 | Kuraray Co Ltd | Polyamide resin composition |
| US6656589B2 (en) * | 2000-12-20 | 2003-12-02 | Mitsui Chemicals, Inc. | Polyamide resin pellet for a miniature part |
| CA2386717A1 (en) * | 2001-05-21 | 2002-11-21 | Kuraray Co., Ltd. | Polyamide composition |
| KR100925301B1 (en) * | 2005-04-08 | 2009-11-04 | 미쓰이 가가쿠 가부시키가이샤 | Flame-retardant polyamide composition |
| CN101875776B (en) * | 2010-03-31 | 2013-03-20 | 深圳市科聚新材料有限公司 | High-strength PPO/PA66 alloy material and preparation method thereof |
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