CN114921095B - High temperature resistant low shrinkage PA10T composition - Google Patents

High temperature resistant low shrinkage PA10T composition Download PDF

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CN114921095B
CN114921095B CN202210741162.5A CN202210741162A CN114921095B CN 114921095 B CN114921095 B CN 114921095B CN 202210741162 A CN202210741162 A CN 202210741162A CN 114921095 B CN114921095 B CN 114921095B
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weight
parts
glass fiber
length
pa10t
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CN114921095A (en
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杨秋会
马茂祥
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Shenzhen Huaying New Material Co ltd
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Shenzhen Huaying New Material Co ltd
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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
    • C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Power Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention provides a PA10T composition with excellent high temperature resistance and good dimensional stability in the processing process and the using process, which comprises PA10T, reinforcing filler, glass fiber, antioxidant, lubricant and other auxiliary agents. The glass fiber with the average length of 400-500 mu m and the length variation coefficient of 0.5-0.7 is introduced into the PA10T composition, so that the dimensional stability of the PA10T in the processing process and the dimensional stability of the PA10T in the use process can be improved to the greatest extent while the high temperature resistance of the PA10T is met, and the requirements of the LED reflective support material on the high temperature resistance and the dimensional stability are met.

Description

High temperature resistant low shrinkage PA10T composition
Technical Field
The invention relates to engineering plastics, in particular to a high-temperature-resistant low-shrinkage polyamide material.
Background
Compared with an incandescent lamp, the LED lamp has the advantages of lower required voltage, small energy consumption, small volume, high effect speed and long service life, and is gradually replaced by the incandescent lamp in many applications, so that the LED lamp is a widely applied light source.
The LED reflecting support needs to be subjected to reflow soldering technology in the processing process, and the requirements on the heat resistance of the material are high. At present, the material capable of meeting the reflow soldering process is mainly semi-aromatic polyamide, such as PA6T, PA9T, PA T and the like. The PA10T has high reflectivity, good dimensional stability and good adhesion with packaging resin, and is widely used for LED reflecting brackets for outdoor display.
With the development of miniaturization of the LED lamp beads year by year, the LED reflecting support is gradually developed towards the small-size direction, fine machining is gradually needed for the support, materials are required to have high heat resistance in the machining process, and good dimensional stability in the machining process and the using process, and therefore higher requirements are set for the heat resistance and the dimensional stability of the PA10T material.
CN104610739a discloses a polyamide composition for an LED reflector, which comprises a compound containing a secondary amine group and a polyamide composition containing phosphorus with a specific content, and can solve the technical problem that the silica gel is not cured completely or even can not be cured in the packaging process of an LED device. CN105602243a discloses a polyamide composition for an LED reflecting support, which not only solves the problem that the whiteness and reflectivity of the LED reflecting support are easy to be reduced when the LED reflecting support is exposed to light and heat, but also can avoid the problem that the silica gel is not cured completely or not cured completely when the polyamide composition is used for a reflecting plate by controlling the mass ratio of magnesium element to phosphorus element in the polyamide composition. CN112724667a discloses a polyamide composition for LED reflective support, and by adding a specific amount of amino-terminated hyperbranched polyamide into the polyamide molding composition, the crystallization temperature, crystallization rate and fluidity of the material can be significantly improved, i.e. the material can have as high a crystallization temperature and a melt index as possible and a minimum peak width at half maximum of crystallization.
None of the above prior art concerns the high temperature resistance and dimensional stability of the material.
Disclosure of Invention
The invention aims to provide a PA10T composition with excellent high temperature resistance and good dimensional stability in the processing process and the using process.
To achieve the above object, the present invention provides a high temperature resistant low shrinkage PA10T composition.
A high temperature resistant low shrinkage PA10T composition comprises PA10T, reinforcing filler, glass fiber, antioxidant, lubricant and other auxiliary agents.
In a preferred embodiment, the composition comprises 100 parts by weight of PA10T, 0-100 parts by weight of reinforcing filler, 5-30 parts by weight of glass fiber, 0-20 parts by weight of antioxidant, 0-20 parts by weight of lubricant and 0-30 parts by weight of other auxiliary agents.
The reinforcing filler is selected from fibrous fillers or powdery fillers, and the reinforcing filler does not comprise glass fibers.
The fibrous filler is selected from one or more of ceramic fiber, basalt fiber, carbon fiber, zinc oxide whisker, calcium sulfate whisker and carbon nano tube.
The powdery filler is selected from one or more of wollastonite, mica, muscovite, talcum, clay, bentonite, montmorillonite, clay, silicon nitride, boron nitride, graphene, graphite, alumina, silica, titanium dioxide, ferroferric oxide, zirconia, calcium carbonate, calcium sulfate, barium sulfate, magnesium hydroxide, calcium hydroxide and aluminum hydroxide.
In a preferred embodiment, the reinforcing filler is 10 to 80 parts by weight, preferably 20 to 50 parts by weight, and more preferably 30 to 40 parts by weight.
The average length of the glass fiber is 400-500 mu m, the average diameter is 7-15 mu m, and the length variation coefficient is 0.5-0.7. Preferably, the glass fiber is prepared by chopping long fiber, and can also be formed by mixing glass fibers with different lengths.
Coefficient of Variation (CV) is a dimensionless parameter that measures the degree of dispersion of a set of data, defined as the ratio of standard deviation to average.
Coefficient of Variation (CV) =standard deviation σ/arithmetic mean μ.
In a preferred embodiment, the average length of the glass fibers is preferably 410 to 490 μm, more preferably 420 μm, 430 μm, 440 μm, 450 μm, 460 μm, 470 μm, 480 μm; the average diameter of the glass fibers is preferably 7 μm, 9 μm, 10 μm, 13 μm, 15 μm; the glass fiber length variation coefficient is preferably 0.55 to 0.65, more preferably 0.6.
In a preferred embodiment, the glass fiber is 10 to 25 parts by weight, preferably 15 to 20 parts by weight, and more preferably 17 parts by weight.
The antioxidant is selected from one or more of hindered phenol antioxidants and phosphite antioxidants, the hindered phenol antioxidants are selected from one or more of antioxidants 1010, 1035, 1330 and 259, and the phosphite antioxidants are selected from one or more of antioxidants 168 and 626 GE. Preferably, the weight ratio of the hindered phenol antioxidant to the phosphite antioxidant is (1-5) to (1-5).
In a preferred embodiment, the antioxidant is preferably 1 to 3 parts by weight, preferably 2 parts by weight.
The lubricant is one or more selected from stearate, stearamide, polyethylene wax and erucamide.
In a preferred embodiment, the lubricant is preferably 1 to 3 parts by weight, preferably 2 parts by weight.
The other auxiliary agents comprise coloring agents, reflective fillers, UV absorbers, anti-aging agents, leveling agents and the like.
In a preferred embodiment, the lubricant is preferably 1 to 25 parts by weight, preferably 5 to 20 parts by weight, preferably 10 to 15 parts by weight.
The invention also provides a preparation method of the high-temperature-resistant low-shrinkage PA10T composition, which comprises the following steps.
The raw materials are added into a high-speed mixer and stirred and mixed uniformly. Adding the mixed materials into a double-screw extruder from a main feeding port of the double-screw extruder, and carrying out melt mixing, extrusion and granulation to obtain the high-temperature-resistant low-shrinkage PA10T composition.
In a preferred embodiment, the rotation speed of the high-speed mixer is 200-2000 rpm, and the mixing time is 5-20 min. The extrusion granulation further comprises the working procedures of extrusion, bracing, cooling, granulating and drying. The processing temperature of the melt mixing is 300-330 ℃.
Compared with the prior art, the invention has the following beneficial effects.
According to the invention, the glass fiber with the average length of 400-500 mu m and the length variation coefficient of 0.5-0.7 is introduced into the PA10T composition, so that the dimensional stability of the PA10T in the processing process and the dimensional stability of the PA10T in the use process can be improved to the greatest extent while the high temperature resistance of the PA10T is met, and the requirements of the LED reflective support material on the high temperature resistance and the dimensional stability are met.
Detailed Description
Further advantages and effects of the present invention will become apparent to those skilled in the art from the disclosure of the present invention, when the following description of the embodiments is taken in conjunction with the accompanying drawings.
Before further describing embodiments of the invention, it is to be understood that the scope of the invention includes, but is not limited to, the following specific embodiments. Generally, the terminology used in the examples of the invention is for the purpose of describing particular embodiments only and is not intended to limit the scope of the invention. The test methods without specific conditions noted in the examples below are generally conducted under conventional conditions or under conditions recommended by the respective manufacturers.
Where numerical ranges are provided in the examples, it is understood that unless otherwise stated herein, both endpoints of each numerical range and any number between the two endpoints are significant both in the numerical range. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In addition to the specific methods, devices, materials used in the embodiments, any methods, devices, and materials of the prior art similar or equivalent to those described in the embodiments of the present invention may be used to practice the present invention according to the knowledge of one skilled in the art and the description of the present invention.
Preparation example
Glass fiber long fibers with the average diameter of 10 μm are selected, cut into short fibers with the set lengths of 300 μm, 350 μm, 400 μm, 450 μm, 500 μm and 550 μm, and glass fiber raw materials GF300, GF350, GF400, GF450, GF500 and GF550 are respectively obtained. The average length and length distribution of the above samples were measured using a fiber length distribution tester, and the results are shown in table 1.
TABLE 1
Example a and comparative example B, C, D
The glass fiber chopped fibers were uniformly mixed in parts by weight as shown in table 2 to obtain mixed glass fibers, and the average length and the length distribution of the samples were measured using a fiber length distribution tester. 20 parts by weight of mixed glass fiber, 100 parts by weight of PA10T, 10 parts by weight of alumina, 10 parts by weight of silicon dioxide, 1010 1 parts by weight of antioxidant, 168 1 parts by weight of antioxidant and 2 parts by weight of polyethylene wax are added into a high-speed mixer, and stirred and mixed for 5min under the condition of 2000 rpm. Adding the mixed materials into a double-screw extruder from a main feeding port of the double-screw extruder, and carrying out melt mixing, extrusion and granulation to obtain the high-temperature-resistant low-shrinkage PA10T composition. The temperature of each zone of the twin-screw extruder is set to 300-330 ℃ and the die opening is set to 310 ℃.
TABLE 2
The above composition was prepared into standard bars, and the melting point, thermal expansion coefficient at 200℃and molding shrinkage were measured, and the results are shown in Table 3.
TABLE 3 Table 3
From the above examples and comparative examples, it can be seen that the average length of the glass fiber staple fibers and the degree of dispersion of the length thereof have a great influence on the high temperature resistance and the dimensional stability of the PA10T material. The applicant obtains a satisfactory glass fiber short fiber composition for PA10T modification by combining short fibers with different lengths after chopping the glass fiber long fibers. It is generally believed that glass fibers having a critical length of 300 μm exhibit some reinforcement beyond this length. It was also found during the staple processing that the shorter glass fiber length distribution was relatively uniform, but as the length increased, the randomness of the glass fiber segment also increased, resulting in a broader glass fiber length distribution. By selecting proper glass fiber short fibers which are formed by the short fibers and meet a certain relation, the high temperature resistance of the PA10T material can be improved, and meanwhile, the dimensional stability in the use process and the dimensional stability in the processing process of the PA10T material can be improved, so that the PA10T can meet the performance requirements of the small-size LED reflecting bracket.
All documents mentioned in this application are incorporated by reference as if each were individually incorporated by reference. Further, it will be appreciated that various changes and modifications may be made by those skilled in the art after reading the above teachings, and such equivalents are intended to fall within the scope of the claims appended hereto.

Claims (6)

1. The high-temperature-resistant low-shrinkage PA10T composition is characterized by comprising 100 parts by weight of PA10T, 20 parts by weight of glass fiber, 10 parts by weight of alumina, 10 parts by weight of silicon dioxide, 1010 parts by weight of antioxidant, 168 parts by weight of antioxidant and 2 parts by weight of polyethylene wax;
the glass fiber is formed by mixing the following glass fibers: 15 parts by weight of GF300, 350 parts by weight of GF350, 400 parts by weight of GF400 and 500 parts by weight of GF500 based on 100 parts by weight of glass fiber;
the GF300 is glass fiber with average length of 294 mu m, length standard deviation of 97 mu m and length variation coefficient of 0.33;
the GF350 is glass fiber with average length of 361 mu m, length standard deviation of 162 mu m and length variation coefficient of 0.45;
the GF400 is glass fiber with the average length of 401 mu m, the length standard deviation of 213 mu m and the length variation coefficient of 0.53;
the GF500 is glass fiber with average length of 518 μm, standard deviation of 332 μm and length variation coefficient of 0.64.
2. The high-temperature-resistant low-shrinkage PA10T composition is characterized by comprising 100 parts by weight of PA10T, 20 parts by weight of glass fiber, 10 parts by weight of alumina, 10 parts by weight of silicon dioxide, 1010 parts by weight of antioxidant, 168 parts by weight of antioxidant and 2 parts by weight of polyethylene wax;
the glass fiber is formed by mixing the following glass fibers: GF400 55 parts by weight, GF450 35 parts by weight, GF500 10 parts by weight, based on 100 parts by weight of glass fiber;
the GF400 is glass fiber with the average length of 401 mu m, the length standard deviation of 213 mu m and the length variation coefficient of 0.53;
the GF450 is glass fiber with the average length of 470 mu m, the length standard deviation of 343 mu m and the length variation coefficient of 0.73;
the GF500 is glass fiber with average length of 518 μm, standard deviation of 332 μm and length variation coefficient of 0.64.
3. The high-temperature-resistant low-shrinkage PA10T composition is characterized by comprising 100 parts by weight of PA10T, 20 parts by weight of glass fiber, 10 parts by weight of alumina, 10 parts by weight of silicon dioxide, 1010 parts by weight of antioxidant, 168 parts by weight of antioxidant and 2 parts by weight of polyethylene wax;
the glass fiber is formed by mixing the following glass fibers: GF350, GF400, GF450, GF500, 100 parts by weight of glass fiber;
the GF350 is glass fiber with average length of 361 mu m, length standard deviation of 162 mu m and length variation coefficient of 0.45;
the GF400 is glass fiber with the average length of 401 mu m, the length standard deviation of 213 mu m and the length variation coefficient of 0.53;
the GF450 is glass fiber with the average length of 470 mu m, the length standard deviation of 343 mu m and the length variation coefficient of 0.73;
the GF500 is glass fiber with average length of 518 μm, standard deviation of 332 μm and length variation coefficient of 0.64.
4. A method for preparing a high temperature resistant low shrinkage PA10T composition according to any one of claims 1-3, comprising the steps of:
adding the raw materials into a high-speed mixer, and uniformly stirring and mixing; adding the mixed materials into a double-screw extruder from a main feeding port of the double-screw extruder, and carrying out melt mixing, extrusion and granulation to obtain the high-temperature-resistant low-shrinkage PA10T composition.
5. The method of claim 4, wherein the melt mixing is performed at a temperature of 300-330 ℃.
6. An LED reflector holder comprising a high temperature resistant low shrinkage PA10T composition according to any one of claims 1-3.
CN202210741162.5A 2022-06-28 2022-06-28 High temperature resistant low shrinkage PA10T composition Active CN114921095B (en)

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CN115260758B (en) * 2022-08-24 2024-01-09 横店集团得邦工程塑料有限公司 High-reflectivity heat aging resistant PA10T material and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101870810A (en) * 2010-03-29 2010-10-27 金发科技股份有限公司 Heat-resistant polyamide composition
WO2013026779A1 (en) * 2011-08-19 2013-02-28 Solvay Specialty Polymers Usa, Llc Improved polyamide compositions for led applications
CN104046000A (en) * 2013-03-15 2014-09-17 上海杰事杰新材料(集团)股份有限公司 Alkali-free short glass fiber reinforced nylon material and preparation method
CN106380837A (en) * 2016-08-31 2017-02-08 上海跃贝塑化科技有限公司 Glass fiber reinforced nylon 6 material with excellent dimensional stability and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101870810A (en) * 2010-03-29 2010-10-27 金发科技股份有限公司 Heat-resistant polyamide composition
WO2013026779A1 (en) * 2011-08-19 2013-02-28 Solvay Specialty Polymers Usa, Llc Improved polyamide compositions for led applications
CN104046000A (en) * 2013-03-15 2014-09-17 上海杰事杰新材料(集团)股份有限公司 Alkali-free short glass fiber reinforced nylon material and preparation method
CN106380837A (en) * 2016-08-31 2017-02-08 上海跃贝塑化科技有限公司 Glass fiber reinforced nylon 6 material with excellent dimensional stability and preparation method thereof

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