CN105602243B - A kind of daiamid composition and its application - Google Patents
A kind of daiamid composition and its application Download PDFInfo
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- CN105602243B CN105602243B CN201510820925.5A CN201510820925A CN105602243B CN 105602243 B CN105602243 B CN 105602243B CN 201510820925 A CN201510820925 A CN 201510820925A CN 105602243 B CN105602243 B CN 105602243B
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- daiamid composition
- magnesium
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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 with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
- H01L33/58—Optical field-shaping elements
- H01L33/60—Reflective elements
-
- 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
Abstract
The invention discloses a kind of daiamid composition and its application, the composition includes：A) the Semi-aromatic polyamide resin of 30 90 parts by weight；B) the white pigment and/or reinforcing filler of 10 50 parts by weight；Wherein, the mass ratio of magnesium elements and P elements is 0.1 100 in the daiamid composition：1.The present invention controls magnesium elements in daiamid composition and P elements mass ratio 0.1 100：In 1 range, the initial whiteness value of daiamid composition is all 90 or more, and its Hunter whiteness value remains to keep 80 or more after aging 4h at 180 DEG C；The daiamid composition is not in the problem of silica gel cures not exclusively or do not cure completely for reflecting plate simultaneously.
Description
Technical field
The invention belongs to polymer modification fields, and in particular to and it is a kind of that there is excellent heat resistance, it is very suitable for answering
For light emitting diode（LED）Reflection holder on daiamid composition.
Background technology
Light-emitting diode LED needs lower voltage, lower, the volume smaller of energy consumption, service life compared with incandescent source
The many advantages such as length, brightness higher, response time be shorter, therefore they are such as handed in many purposes instead of incandescent source
Messenger, inside and outside illumination, mobile phone display screen, automobile display screen and flash lamp.
LED component, if shell, reflector and reflector panel require to possess excellent color and physical characteristic, although pottery
Porcelain can be advantageously applied to this, but ceramics treatment technology that is extremely expensive and needing high request.However polymer composition has
There is relatively low cost, and can be by injection molding difference looking products, therefore, scientific research personnel carries out polymer composition
Extensive research is to replace ceramics.
Application of the polymer composition on LED, it is desirable that it is with good opaqueness and excellent reflection characteristic；It needs simultaneously
Pay special attention to problems with, LED component can be exposed under light and hot environment during manufacturing process or use, be easy to lead
It causes jaundice and influences its reflecting effect to light.For example following manufacturing process is worth note that LED components need to be heated to 180 DEG C of left sides
The right side is so as to cured epoxy resin or silicon encapsulant；When carrying out SMT (surface mount), LED components can be exposed on higher than 260
At a temperature of DEG C；In addition, in use, if LED components are used for automobile, to be subjected to higher than 80 DEG C of temperature for a long time.
In LED encapsulation process, LED component need to be heated to certain temperature so that silica gel cures, this is that LED encapsulation must can not
Few link and vital link.The study found that it is easy to appear silica gel to cure not exclusively even in this process
The problem of not curing completely causes the production process in later stage that can not carry out, and product can not use.
In summary, LED reflection holder whiteness and reflectivity when being exposed in light and heat are easy to decline, and follow-up
The problem of silica gel solidification does not cure even not exclusively completely is susceptible in encapsulation process, and in the prior art for the above problem
And the technical solution to solve the above problems rarely has and refers to.
The present inventor pass through many experiments surprisingly it has been found that, pass through and control magnesium elements and P elements matter in daiamid composition
Ratio is measured, not only solves the problems, such as that LED reflection holder whiteness and reflectivity when being exposed in light and heat are easy decline, and simultaneously can
Avoid the problem that daiamid composition silica gel solidification occurs for reflecting plate and do not cure not exclusively or completely.
Invention content
The purpose of the present invention is to provide a kind of daiamid compositions, pass through magnesium elements in control composition and P elements matter
Ratio is measured, can not only realize high whiteness, moreover it is possible to while realizing later stage silica gel completion of cure.
The present invention is achieved by the following technical solutions：
A kind of daiamid composition, including following component：
A) the Semi-aromatic polyamide resin of 30-90 parts by weight；
B) the white pigment and/or reinforcing filler of 10-50 parts by weight；
Wherein, the mass ratio of magnesium elements and P elements is 0.1-100 in the daiamid composition：1, the magnesium elements and phosphorus
The mass ratio of element is according to USEPA methods 3052:1996, it is measured using ICP-AES methods.
The mass ratio of magnesium elements and P elements is preferably 2-60 in the wherein described daiamid composition:1, more preferably 10-
35:1。
The wherein described Semi-aromatic polyamide resin, with reference to ASTM D3418-2003, using Perkin Elmer
Diamond dsc analysis instrument, in nitrogen atmosphere, flow velocity 40mL/min, when test, is first warming up to 340 DEG C with 10 DEG C/min,
340 DEG C of holding 2min, are then cooled to 50 DEG C, then be warming up to 10 DEG C/min and measured under conditions of 340 DEG C with 10 DEG C/min
Fusing point is more than 280 DEG C；
The wherein described Semi-aromatic polyamide resin, according to 11443 methods of ISO, using capillary rheometer LCR7000,
Outflux angle be 120o, 1.2 inches of flow channel length, 0.03 inch of flow diameter, test temperature be fusing point [（Tm）+10]
DEG C, melting time 300s, shear rate 1000s-1Under conditions of measure its melt viscosity be 50-400Pa.s.
The wherein described Semi-aromatic polyamide resin by the aliphatic diamine of 3-36 carbon atom, aromatic diacid or/and
The unit that aliphatic diacid is formed is constituted；The wherein aliphatic diamine of the preferred 6-10 carbon atom of aliphatic diamine, more preferable 9 or
The aliphatic diamine of 10 carbon atoms.The polyamide that the aliphatic diamine of 9 or 10 carbon atoms is prepared, water absorption rate is lower,
Be conducive to ageing-resistant performance.
Wherein the white pigment is selected from titanium dioxide, zinc oxide, zinc sulphide, white lead, zinc sulfate, barium sulfate, carbonic acid
It is one or more in calcium, aluminium oxide.
Wherein the reinforcing filler includes one or more in threadiness, tabular, needle-shaped reinforcing filler, wherein
Fibrous reinforced filler is glass fibre, carbon fiber, aramid fibre, liquid crystal polymer (LCP) fiber, metallic fiber
In it is one or more；Tabular reinforcing filler is one kind or combinations thereof in mica or talcum powder；Needle-shaped reinforcing filler is titanium
Sour potassium whisker, aluminium borate whisker, calcium carbonate crystal whisker, wollastonite, sepiolite, eakleite, one kind in ZnOw or more
Kind.
Preferably, reinforcing filler can also include silica, aluminium oxide, barium carbonate, aluminium nitride, boron nitride, potassium titanate,
Kaolin, clay, pyrophillite, bentonite, calcium silicates, attapulgite, aluminium borate, calcium sulfate, barium sulfate, asbestos, bead, stone
Ink, carbon nanotube, silicon carbide, sericite, hydrotalcite, molybdenum disulfide, phenolic resin, cross-linked styrene system resin, crosslink propylene
It is one or more in acid system resin.
Wherein the magnesium elements come from magnesium-containing compound, selected from magnesia, magnesium hydroxide, magnesium chloride, magnesium sulfate, silicic acid
It is one or more in magnesium, magnesium carbonate, magnesium nitrate.
Wherein the P elements come from phosphorus-containing compound, selected from potassium phosphate, sodium phosphate, potassium dihydrogen phosphate, biphosphate
One kind or combinations thereof in sodium, phosphate, phosphite ester, Sodium Acid Pyrophosphate.
Preferably, can also be further included in daiamid composition the polytetrafluoroethylene (PTFE) of 0-10 parts by weight, polyolefins,
Ethylene-propylene copolymer, ethylene-butene-1 copolymer, propene-1-butene copolymer, polystyrene type, fatty polyamide,
One kind or combinations thereof in makrolon, polyacetals, polysulfones, polyphenylene oxide, fluororesin, silicone resin, liquid crystal polymer (LCP).
According to different purposes needs, polyamide compositions species of the invention can further include 0-10 parts by weight
Antioxidant, light stabilizer, impact modifier, fire retardant, fluorescent whitening agent, lubricant, plasticizer, thickener, antistatic agent,
It is one or more in releasing agent, pigment.
Compared with prior art, the present invention having the advantages that：
By many experiments, surprisingly it has been found that, the present invention controls magnesium elements in daiamid composition and P elements mass ratio
Within the scope of 0.1-1000, the initial whiteness value of daiamid composition all 90 or more, and through aging 4h at 180 DEG C it
Its Hunter whiteness value remains to keep 80 or more afterwards；The daiamid composition is not in silica gel solidification for LED reflector plate simultaneously
The problem of not exclusively or not curing completely.
Description of the drawings
The assay maps of required daiamid composition when Fig. 1 is silica gel solidification test.
Specific implementation mode
It is further illustrated the present invention below by specific implementation mode, following embodiment is the preferable embodiment party of the present invention
Formula, but embodiments of the present invention are not limited by following embodiments.
Polyamide：
High temperature resistant nylon comes from JinFa Science Co., Ltd (Kingfa Sci. ＆ Tech. Co., Ltd),
Melt viscosity, using capillary rheometer LCR7000, is fusing point in temperature according to 11443 methods of ISO（Tm）+ 10 DEG C, shearing
It is tested under rate 1000s-1；
Reinforcing filler
Glass fibre：From OWENS CORNING composite material company (OCVTM Reinforcements) commercially available glass
Fiber OCV 995.
White pigment
Titanium dioxide：From Ishihara Sangyo Kaisha, Ltd. (Ishihara Sangyo Kaisha) commercially available PC-3 by chlorine
The rutile TiO2 of compound method manufacture.
Phosphorus-containing compound
Phosphorus-containing compound 1：Ultranox626 be phosphite ester --- (2,4- di-tert-butyl-phenyl) pentaerythrite
Diphosphites, commercially available from Chemtura Corporation (Chemtura).
Phosphorus-containing compound 2：Sodium Acid Pyrophosphate, commercially available from the bio tech ltd Zhong Xu of Anhui.
Magnesium-containing compound
Magnesia, commercially available from the Rui Yu photoelectric materials Co., Ltd of Shanghai.
Lubricant
Lubricant：From the PED191 commercially available from AmeriLubes, L.L.C, a kind of polyethylene wax of the oxidation of high molecular weight.
LED packaging silicon rubbers：LED packaging silicon rubbers commercially available from the Yong Xinren Science and Technology Ltd.s of Shenzhen, UH-6950-1（AB
Glue）.
The method for preparing composition
Using homogenizer by dried Semi-aromatic polyamide resin and magnesium-containing compound, phosphorus-containing compound, profit
Lubrication prescription etc. is uniformly mixed, and is added from twin-screw extrusion owner's spout, titanium dioxide is added with glass fibre by side feeder
Enter double screw extruder, by double screw extruder melting extrusion, granulation at a temperature of 230-330 DEG C of setting, obtains granular
Daiamid composition；Then by obtained particulate polymeric composition in 120 DEG C of removal moisture drying 5h, in 260-335 DEG C of setting
At a temperature of, it is prepared for the sample needed for related whiteness and silica gel solidification test by injection molding.Each component matches when property
Energy
Test result is as shown in table 1-3.
Measurement method
（1）Hunter whiteness（W）Test
Use Color Eye 7000A type colorimeter measurements.The daiamid composition sample uses injection molding, sample
Size is 60 × 60 × 0.8mm.L, a, b value for testing out sample original state calculate initial whiteness by formula 1
Value, then sample is kept measuring its L, a, b value again after 4h under conditions of 180 DEG C of temperature, aging is calculated by formula 1
Hunter whiteness value afterwards, the decline of whiteness value is evaluated with this.
（Formula 1）
（2）Fusing point（Tm）Test
Polyester resin fusing point（Tm）Test is with reference to ASTM D3418-2003, Standard Test Method for
Transition Temperatures of Polymers By Differential Scanning Calorimetry；Specifically
Test method is：Using the fusing point of Perkin Elmer Diamond dsc analysis instrument test samples；Nitrogen atmosphere, flow velocity are
40mL/min；340 DEG C first are warming up to 10 DEG C/min when test, 2min is kept at 340 DEG C, is then cooled to 10 DEG C/min
50 DEG C, then 340 DEG C are warming up to 10 DEG C/min, endotherm peak temperature at this time is set as fusing point Tm.
（3）Silica gel solidification test
The daiamid composition particle injection molding of gained is become into sample as shown in Figure 1.By silica gel A glue and B glue with quality
Than 1:4 after mixing, and 0.02g is taken to drop in the pit of exemplar upper surface, so that layer of silica gel is laid in hole bottom, then puts exemplar
Enter in baking oven, precuring 1h under the conditions of 80 DEG C, is then warming up to 150 DEG C and continues to terminate after curing 4h.Tablet is taken out, with the naked eye
The silica gel directly observed in pit cures situation.It is fully cured and is expressed as " ⊙ ", do not cure and be expressed as "×".
（4）Melt viscosity is tested
According to 11443 methods of ISO, using capillary rheometer LCR7000, the polyamide resin is tested using the following conditions
The melt viscosity of fat：Used example weight about 50g, CX300-40, outflux angle is 120 DEG C, 1.2 English of flow channel length
Very little, 0.03 inch of flow diameter, test temperature is (Tm+10) DEG C, melting time 300s.
（5）Magnesium elements and P elements mass ratio
According to USEPA methods 3052:1996, it is measured using ICP-AES methods, obtains magnesium member in daiamid composition
Cellulose content and phosphorus element content, to obtain magnesium elements and P elements mass ratio.
The proportioning of 1 embodiment 1-9 each components of table（Parts by weight）And the performance test results
The proportioning of 2 embodiment 10-18 each components of table（Parts by weight）And the performance test results
The proportioning of 3 comparative example 1-4 each components of table（Parts by weight）And the performance test results
Magnesium in daiamid composition/phosphorus mass ratio is can be seen that in 0.1-100 ranges from the embodiment 1-18 of Tables 1 and 2
Interior, the initial whiteness value of daiamid composition is all 90 or more, and its Hunter whiteness value after aging 4h at 180 DEG C
It remains to keep 80 or more；There is not silica gel solidification not in later stage silica gel cures test process in these daiamid compositions simultaneously
The problem of not curing entirely or entirely.
It can be seen that by the comparative example 1-4 of table 3 when magnesium/phosphorus weight ratio is less than 0.1 in daiamid composition, polyamides
Although the initial whiteness value of amine composition can be more than 90, its Hunter whiteness value can be less than after aging 4h at 180 DEG C
80；And there is the problem of silica gel cures not exclusively or do not cure completely in later stage silica gel cures test process.When polyamide group
Close object in magnesium/phosphorus weight ratio be more than 100 when, although later stage silica gel cure test process in do not occur silica gel solidification not exclusively or
The problem of not curing completely, and the initial whiteness value of daiamid composition also can be 90 or more, but through aging 4h at 180 DEG C
Its Hunter whiteness value is much smaller than 80 later.
Claims (14)
1. a kind of daiamid composition, which is characterized in that including following component：
A) the Semi-aromatic polyamide resin of 30-90 parts by weight；
B) the white pigment and reinforcing filler of 10-50 parts by weight；
Wherein, the mass ratio of magnesium elements and P elements is 0.1-100 in the daiamid composition：1；
The magnesium elements come from magnesium-containing compound, selected from magnesia, magnesium hydroxide, magnesium chloride, magnesium sulfate, magnesium silicate, magnesium carbonate,
It is one or more in magnesium nitrate；
The P elements come from phosphorus-containing compound, selected from potassium phosphate, sodium phosphate, potassium dihydrogen phosphate, sodium dihydrogen phosphate, phosphate,
One kind or combinations thereof in phosphite ester, Sodium Acid Pyrophosphate;
The reinforcing filler includes one or more in threadiness, tabular, needle-shaped reinforcing filler, wherein threadiness increases
Strong filler is one kind or more in glass fibre, carbon fiber, aramid fibre, liquid crystal polymer fibre or metallic fiber
Kind；Needle-shaped reinforcing filler is potassium titanate crystal whisker, aluminium borate whisker, calcium carbonate crystal whisker, wollastonite, eakleite or ZnOw
In it is one or more;
The reinforcing filler further includes silica, aluminium oxide, barium carbonate, aluminium nitride, boron nitride, calcium silicates, calcium sulfate, sulphur
Sour barium, bead, graphite, carbon nanotube, silicon carbide, molybdenum disulfide, phenolic resin, cross-linked styrene system resin or crosslink propylene
It is one or more in acid system resin.
2. daiamid composition according to claim 1, which is characterized in that the mass ratio of the magnesium elements and P elements
According to USEPA methods 3052:1996, it is measured using ICP-AES methods.
3. daiamid composition according to claim 1, which is characterized in that magnesium elements and phosphorus in the daiamid composition
The mass ratio of element is 2-60:1.
4. daiamid composition according to claim 3, which is characterized in that magnesium elements and phosphorus in the daiamid composition
The mass ratio of element is 10-35:1.
5. daiamid composition according to claim 1, which is characterized in that the fusing point of the Semi-aromatic polyamide resin
More than 280 DEG C, with reference to ASTM D3418-2003, using Perkin Elmer Diamond dsc analysis instrument, in nitrogen atmosphere,
Flow velocity is 40mL/min, and when test is first warming up to 340 DEG C with 10 DEG C/min, 2min is kept at 340 DEG C, then with 10 DEG C/min
It is cooled to 50 DEG C, then is warming up to 10 DEG C/min and is measured under conditions of 340 DEG C；
The melt viscosity of the Semi-aromatic polyamide resin is that 50-400Pa.s uses capillary according to 11443 methods of ISO
Rheometer LCR7000, outflux angle is 120o, 1.2 inches of flow channel length, 0.03 inch of flow diameter, test temperature are
Fusing point [（Tm）+ 10] DEG C, melting time 300s, shear rate 1000s-1Under conditions of measure.
6. daiamid composition according to claim 5, which is characterized in that the Semi-aromatic polyamide resin is by 3-36
The unit that the aliphatic diamine and aromatic diacid of a carbon atom are formed is constituted.
7. daiamid composition according to claim 6, which is characterized in that the aliphatic diamine is 6 or 10 carbon originals
The aliphatic diamine of son.
8. daiamid composition according to claim 7, which is characterized in that the aliphatic diamine is 9 or 10 carbon originals
The aliphatic diamine of son.
9. daiamid composition according to claim 1, which is characterized in that the white pigment be selected from titanium dioxide,
It is one or more in zinc oxide, zinc sulphide, white lead, zinc sulfate, barium sulfate, calcium carbonate, aluminium oxide.
10. daiamid composition according to claim 1, which is characterized in that the daiamid composition also includes 0-10
In the polyolefins of parts by weight, fatty polyamide, makrolon, polyacetals, polysulfones, polyphenylene oxide, fluororesin, silicone resin
One kind or combinations thereof.
11. daiamid composition according to claim 10, which is characterized in that the fluororesin is polytetrafluoroethylene (PTFE), institute
It is ethylene-propylene copolymer, ethylene-butene-1 copolymer or propene-1-butene copolymer to state polyolefins.
12. daiamid composition according to claim 1, which is characterized in that the daiamid composition further includes 0-10
The antioxidants of parts by weight, light stabilizer, impact modifier, fire retardant, fluorescent whitening agent, lubricant, plasticizer, thickener,
It is one or more in antistatic agent, releasing agent.
13. according to claim 1-12 any one of them daiamid compositions, which is characterized in that the daiamid composition
Initial whiteness value is more than 90, its Hunter whiteness value is 80 or more after keeping 4h under 180 DEG C of temperature condition.
14. application of the claim 1-13 any one of them daiamid compositions in LED reflector plate.
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| JP7412337B2 (en) | 2017-12-19 | 2024-01-12 | ビーエーエスエフ ソシエタス・ヨーロピア | Stabilizer compositions, methods of use thereof, and plastic compositions containing the stabilizer compositions. |
| CN110922749A (en) * | 2019-10-26 | 2020-03-27 | 张家港大塚化学有限公司 | Preparation method of high-weather-resistance and high-reflectivity polyamide composite material for LED |
| CN111748200A (en) * | 2020-07-14 | 2020-10-09 | 中广核瑞胜发（厦门）新材料有限公司 | Heat-conducting flame-retardant nylon composite material with improved cold and thermal shock resistance and preparation method thereof |
| CN112662172B (en) * | 2020-12-09 | 2022-10-18 | 珠海万通特种工程塑料有限公司 | Semi-aromatic polyamide resin composition and preparation method and application thereof |
| CN114591624B (en) * | 2022-03-17 | 2023-06-20 | 珠海万通特种工程塑料有限公司 | Gray semi-aromatic polyamide molding composition and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104145347A (en) * | 2012-02-28 | 2014-11-12 | 东洋纺株式会社 | Thermoplastic resin composition for led reflector plates |
| CN104610739A (en) * | 2015-01-21 | 2015-05-13 | 金发科技股份有限公司 | Polyamide composition for reflective plate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20120165448A1 (en) * | 2010-12-28 | 2012-06-28 | Cheil Industries Inc. | Polyamide Resin Composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104145347A (en) * | 2012-02-28 | 2014-11-12 | 东洋纺株式会社 | Thermoplastic resin composition for led reflector plates |
| CN104610739A (en) * | 2015-01-21 | 2015-05-13 | 金发科技股份有限公司 | Polyamide composition for reflective plate |
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