CN114685977B - Polyamide molding composition and application thereof - Google Patents
Polyamide molding composition and application thereof Download PDFInfo
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- CN114685977B CN114685977B CN202011588443.9A CN202011588443A CN114685977B CN 114685977 B CN114685977 B CN 114685977B CN 202011588443 A CN202011588443 A CN 202011588443A CN 114685977 B CN114685977 B CN 114685977B
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- 239000004952 Polyamide Substances 0.000 title claims abstract description 40
- 239000000203 mixture Substances 0.000 title claims abstract description 40
- 238000000465 moulding Methods 0.000 title claims abstract description 40
- 229920002647 polyamide Polymers 0.000 title claims abstract description 40
- 229920006111 poly(hexamethylene terephthalamide) Polymers 0.000 claims abstract description 40
- 239000010456 wollastonite Substances 0.000 claims abstract description 31
- 229910052882 wollastonite Inorganic materials 0.000 claims abstract description 31
- 238000002310 reflectometry Methods 0.000 claims abstract description 9
- 229920005989 resin Polymers 0.000 claims description 19
- 239000011347 resin Substances 0.000 claims description 19
- 239000003963 antioxidant agent Substances 0.000 claims description 16
- JZUHIOJYCPIVLQ-UHFFFAOYSA-N 2-methylpentane-1,5-diamine Chemical group NCC(C)CCCN JZUHIOJYCPIVLQ-UHFFFAOYSA-N 0.000 claims description 11
- 125000004427 diamine group Chemical group 0.000 claims description 7
- 230000003078 antioxidant effect Effects 0.000 claims description 6
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical group NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 6
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical group OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 6
- KKEYFWRCBNTPAC-UHFFFAOYSA-N terephthalic acid group Chemical group C(C1=CC=C(C(=O)O)C=C1)(=O)O KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 239000006229 carbon black Substances 0.000 claims description 3
- 150000004985 diamines Chemical class 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- ODJQKYXPKWQWNK-UHFFFAOYSA-L 3-(2-carboxylatoethylsulfanyl)propanoate Chemical compound [O-]C(=O)CCSCCC([O-])=O ODJQKYXPKWQWNK-UHFFFAOYSA-L 0.000 claims description 2
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 5
- 239000004033 plastic Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000012858 packaging process Methods 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract 2
- 230000007774 longterm Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 16
- VSGPGYWZVPDDSK-UHFFFAOYSA-N 2-(5-methoxy-2-phenyl-1h-indol-3-yl)-n,n-dimethylethanamine Chemical compound CN(C)CCC=1C2=CC(OC)=CC=C2NC=1C1=CC=CC=C1 VSGPGYWZVPDDSK-UHFFFAOYSA-N 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 15
- 238000012360 testing method Methods 0.000 description 11
- 235000006708 antioxidants Nutrition 0.000 description 9
- 239000012466 permeate Substances 0.000 description 7
- 229920006131 poly(hexamethylene isophthalamide-co-terephthalamide) Polymers 0.000 description 7
- 229920006117 poly(hexamethylene terephthalamide)-co- polycaprolactam Polymers 0.000 description 7
- 239000011324 bead Substances 0.000 description 5
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000005227 gel permeation chromatography Methods 0.000 description 4
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 3
- 238000001746 injection moulding Methods 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- BYEAHWXPCBROCE-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropan-2-ol Chemical compound FC(F)(F)C(O)C(F)(F)F BYEAHWXPCBROCE-UHFFFAOYSA-N 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000001579 optical reflectometry Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- APTZNLHMIGJTEW-UHFFFAOYSA-N pyraflufen-ethyl Chemical compound C1=C(Cl)C(OCC(=O)OCC)=CC(C=2C(=C(OC(F)F)N(C)N=2)Cl)=C1F APTZNLHMIGJTEW-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 210000001525 retina Anatomy 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a polyamide molding composition which can be used for producing LED reflecting brackets, mainly by selecting PA6T/X of specific repeating units, regulating whiteness to be less than 30 by using toner and wollastonite, regulating light source reflectivity of 460nm to be less than 8 percent, and the like. The polyamide molding composition has the advantage of good adhesion between plastic and hardware, and can be applied to the LED display screen light source reflection bracket to promote the LED display screen to have the advantages of high contrast, high gray level and blue light reduction, so that the requirements of a packaging process and long-term use reliability can be met, and the packaged product can be used for manufacturing the high-contrast LED display screen light source reflection bracket for multi-scene application.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a polyamide molding composition and application thereof.
Background
The LED light source mainly comprises a semiconductor chip, an LED light source reflecting support, gold wires and packaging adhesive. The LED light source reflection support is a 'skeleton' of an LED light source and is also a functional piece. The LED packaging process needs to be solidified through die bonding, bonding wires and packaging glue, and other materials and components are integrated. The LED reflection bracket needs to reflect the light emitted by the LED chip through a certain angle, reduces light loss, and then forms a light source for LED illumination or display through packaging materials such as epoxy resin or silica gel. The LED reflective support material is a core material of LED illumination, and is directly related to the performance and service life of an LED light source.
At present, the following points need to be considered in the selection of the materials of the LED reflecting support:
firstly, in the whole packaging process, the LED reflecting support needs to be exposed for 6-10 hours at the temperature of 150-200 ℃, meanwhile, when the packaged lamp beads are manufactured into a display screen, SMT is needed, the LED support or the lamp beads are required to be packaged and SMT, deformation cannot occur, the LED support or the lamp beads are not damaged under the condition of loading, and the requirements on heat resistance and mechanical strength of the LED support material are high.
Second, LED display light sources have been gradually developed in recent years toward small pitch displays with a dot pitch below P2.5, so that LED display development and manufacturing have also been continually challenged in this process. The manufacturing of the small-space display screen bracket gradually develops towards thin walls, multiple cavities and small sizes, and more stringent requirements are put on the flowability, the super-cavity formability, the mechanical strength and the like of the LED reflective bracket material.
Thirdly, in the use process of the LED lamp or the display screen, due to different environments, the LED lamp or the display screen is often influenced by severe weather such as high temperature, typhoon, storm, thunderbolt and the like, and the lamp or the display screen is required to be safe and safe in severe weather, so that the light source failure in various environments is prevented, and the requirements on the adhesion of plastic used by the LED reflecting support and hardware are high.
Fourth, in the field of LED display applications, brightness and contrast of a display screen are very important indicators for displaying sharp and clear image quality. At present, more schemes are mainly used in the market, namely, an LED bracket produced by a pure white LED reflecting material, black printing ink is needed on the surface of the LED bracket, the procedures are complicated, the efficiency is influenced, the cost is high, but the side surface and the surface of a reflecting cup are still white, and the contrast and the gray level displayed by an LED display screen are reduced.
Fifth, regarding the light source: in one aspect, the wavelength that can be perceived by the human eye is between 780 and 400 nm. Wherein blue light is light having a wavelength between 400nm and 480 nm. Short-wave blue light with the wavelength of 400-450 nm has the greatest damage degree on retina, and the blue light with the wavelength can increase the toxin amount of a macular region in eyes, thereby seriously threatening the eye health of people. On the other hand, the LED full-color display screen light source is formed by packaging three chips of red (R), green (G) and blue (B), wherein the brightness of the blue light chip for light emission is the lowest, namely the contrast ratio is the highest, so that the LED light source support can directly influence the degree of the highest contrast ratio of the whole LED display screen for the blue light reflectivity of the chip. The blue light prevention of the LED screen is commonly used for LED screens of various mobile phones and televisions, but the common measure is to coat a blue light prevention film on the surface of the screen, but the measure has the defects of fragile film and high cost respectively.
Those skilled in the art have focused on improvements in the LED reflective support material on the first and second points described above. The problem of the adhesion between the materials used for the LED support and the hardware of the support is rarely related, and the contrast ratio and the gray level of the LED display screen support are improved, and the blue light is reduced.
Disclosure of Invention
The invention aims to provide a polyamide molding composition which has the advantage of good adhesion with hardware, and can be applied to an LED display screen bracket to enable the LED display screen to have the advantages of high contrast ratio and high gray level.
It is a further object of the present invention to provide the use of the polyamide molding composition described above.
The invention is realized by the following technical scheme:
a polyamide molding composition comprises the following components in parts by weight:
40-70 parts of PA6T/X resin;
30-60 parts of wollastonite;
0.4-5 parts of toner;
based on the mole percent of PA6T/X, the content of 6T units is 50-70mol percent, and the content of X units is 30-50mol percent;
wherein the X unit consists of a diacid unit and a diamine unit, the diacid unit comprises one or a combination of more of terephthalic acid unit and isophthalic acid unit, and the diamine unit comprises 1, 6-hexamethylenediamine unit and/or 2-methyl-1, 5-pentanediamine unit;
wollastonite has an average diameter of 4 to 20 μm and an average length of 10 to 250 μm in the polyamide molding composition;
the whiteness of the polyamide molding composition is less than 30, and the light source reflectivity of 460nm is less than 8%.
Preferably, the wollastonite content is 40-55 parts.
The 6T/X ratio is preferably, based on the PA6T/X mole percent, from 50 to 60mol% of 6T units and from 40 to 50mol% of X units.
In the polyamide repeating unit formula: t of the diacid represents terephthalic acid, I represents isophthalic acid, 6 of the diamine represents 1, 6-hexamethylenediamine, MPD represents 2-methyl-1, 5-pentanediamine.
Further, the X unit is preferably selected, and the PA6T/X has a 2-methyl-1, 5-pentanediamine content of 20 to 100mol% in the diamine unit based on the mole percentage of the X unit.
Still preferably, in the PA6T/X, the 2-methyl-1, 5-pentanediamine in the diamine unit accounts for 60 to 100mol% based on the mole percentage of the X unit.
More preferably, the diamine of the X unit in the PA6T/X is 2-methyl-1, 5-pentanediamine.
The number average molecular weight of the PA6T/X resin which can achieve the object of the present invention is in the range of 1000 to 300000.
The PA6T/X resin of the invention can be a commercial product or can be synthesized according to the following method:
(1) Prepolymerization: polymerization monomers (hexamethylenediamine, 2-methyl-1, 5-pentanediamine, terephthalic acid, isophthalic acid, etc.), a capping agent benzoic acid, and deionized water were charged into a stainless steel autoclave equipped with mechanical stirring. Vacuum is applied and N is used 2 Heating and stirring are started after three times of replacement, the temperature is raised to 180 ℃ at the heating rate of 5 ℃/min, the temperature is kept constant for 60min, the temperature is slowly stirred and kept constant for 4 h at the heating rate of 270 ℃ at the heating rate of 2 ℃/min, and the prepolymerization reaction is fully carried outAnd (3) row. After the constant temperature is over, the temperature is slowly increased to 280 ℃, and water drainage is started to normal pressure. And after the pressure is reduced to normal pressure, closing the drain valve, ending the reaction, and discharging after the temperature is reduced to room temperature.
(2) Solid phase tackifying: the material prepared in the prepolymerization process was fed into a vacuum drum, the drum speed was set at 10 r/min and the vacuum was set at 30 Pa. Heating at a speed of 20 ℃/min, sampling and testing the viscosity when the temperature reaches 265 ℃, and judging the discharging end point according to the viscosity result.
Preferably, the wollastonite has an average diameter in the polyamide molding composition of 7 to 15. Mu.m, and an average length of 80 to 160. Mu.m. It was found through experimentation that wollastonite showed no significant decrease in diameter and length at high temperature, high shear conditions in a twin screw extruder.
The toner is selected from carbon black, black seeds or mixed toner with various colors.
Preferably, the toner is selected from non-oriented carbon toners.
Preferably, the 460nm light source has a reflectance of less than 6%, more preferably 3-5%.
The anti-oxidant also comprises 0-3 parts by weight of an anti-oxidant; the antioxidant is at least one selected from hindered phenol antioxidants, hindered amine antioxidants, phosphite antioxidants, mercaptan antioxidants and thiodipropionate antioxidants.
The polyamide molding composition of the invention is used for preparing LED light source reflection brackets.
The invention has the following beneficial effects:
the reflectivity of the 460nm light source is mainly related to the surface roughness of the material (the larger the roughness of the surface of the object is within a certain range, the diffuse reflection of the light emitted by the light source on the surface of the object is generated, and finally, the less the energy of the light received by the light receiving end is), and the whiteness of the material (the lower the whiteness is, the lower the reflectivity is). The influence of the light source reflection bracket of the LED display screen on the gray scale and the contrast of the LED display screen is mainly related to the whiteness and the reflectivity of the light source reflection bracket. According to this principle, the polyamide molding composition of the present invention controls the reduction of the reflectance of a light source having whiteness of < 30 and 460nm to < 8% (improvement of gray scale and contrast), and has the advantages of good adhesion to hardware, and low blue light of the packaged LED screen.
1. Compared with other inorganic fillers, wollastonite can enable the surface roughness of the polyamide molding composition to reach a reasonable range for reducing light reflection, so that the light source reflectivity of 460nm is reduced, and the adhesion with hardware is improved. The preferable distribution size of wollastonite in the resin matrix can further reduce the reflectance of the 460nm light source (reduce blue light of the LED display screen) and improve the adhesion with hardware.
2. The black light absorption effect is good through the color of the toner condition material, and the optimized non-oriented carbon toner can further reduce whiteness and improve light absorption, so that the light source reflectivity of 460nm is reduced.
3. The special repeating unit structure of the PA6T/X resin is cooperated with wollastonite to further improve the adhesion between the surface roughness plating and hardware, and the addition amount of the toner can be reduced.
4. The polyamide molding composition does not need to be additionally sprayed with light-absorbing paint or frosted, so that the cost of the LED display screen light source reflection bracket is reduced.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present invention.
The raw materials used in the examples and comparative examples are as follows:
PA6T 6I resin: the content of X units is 50mol%, the number average molecular weight is 8300, and the preparation is self-made.
PA6T resin: the content of X units is 50mol%, the number average molecular weight is 8100, and the self-made product is prepared.
PA6T/6T MPDT resin-1: the content of the X unit is 50mol%, the proportion of MPD repeating units in the X unit is 10mol%, and the number average molecular weight is 11600;
PA6T/6T MPDT resin-2: the content of the X unit is 50mol%, the proportion of MPD repeating units in the X unit is 20mol%, and the number average molecular weight is 8900;
PA6T/6T MPDT resin-3: the content of the X unit is 50mol%, the proportion of MPD repeating units in the X unit is 40mol%, and the number average molecular weight is 9700;
PA6T/6T MPDT resin-4: the content of the X unit is 50mol%, the proportion of MPD repeating units in the X unit is 60mol%, and the number average molecular weight is 8200;
PA6T/6T MPDT resin-5: the content of the X unit is 50mol%, the proportion of MPD repeating units in the X unit is 80mol%, and the number average molecular weight is 13500;
PA 6T/MPDT resin: the X unit content was 50mol% and the number average molecular weight was 7900.
PA6T/6 IMPDI resin-1: the content of the X unit is 50mol%, the proportion of MPD repeating units in the X unit is 10mol%, and the number average molecular weight is 11200;
PA 6T/6I MPDI resin-2: the content of X units is 50mol%, the proportion of MPD repeating units in the X units is 60mol%, and the number average molecular weight is 9800.
PA 6T/6I MPDI resin-3: the content of X units was 40mol%, the proportion of MPD repeating units in the X units was 60mol%, and the number average molecular weight was 9500.
PA 6T/6I MPDI resin-4: the content of X units is 30mol%, the proportion of MPD repeating units in the X units is 60mol%, and the number average molecular weight is 10600.
PA 6T/6I MPDI resin-5: the content of X units is 20mol%, the proportion of MPD repeating units in the X units is 60mol%, and the number average molecular weight is 8000.
PA 6T/6I MPDI resin-6: the content of X units is 60mol%, the proportion of MPD repeating units in the X units is 60mol%, and the number average molecular weight is 7600.
Wollastonite a: the average diameter is 13 μm and the average length is 80 μm;
wollastonite B: average diameter of 8 μm and average length of 150 μm;
wollastonite C: average diameter of 4 μm and average length of 60 μm;
wollastonite D: the average diameter was 20. Mu.m, and the average length was 210. Mu.m.
Talc powder: AH-1250, guangxi Longshenghuamei Talc development Co., ltd.
Toner a: non-directional carbon toner N774, tianjin day Yang Qiu, chemical technology limited;
toner B: carbon black M570, cabo chemical company, inc;
toner C: black UN2014, cabo chemical limited.
Preparation of the polyamide moulding compositions of examples and comparative examples: adding PA6T/X resin, wollastonite, toner and antioxidant into a mixer, uniformly mixing, and extruding and granulating by a double-screw extruder to obtain a polyamide molding composition; wherein the temperature range of the screw is 280-330 ℃ and the rotating speed is 450r/min.
The testing method comprises the following steps:
(1) Number average molecular weight: the weight average molecular weight (Mw) and number average molecular weight (Mn) of the PA6T/X resin samples were determined by gel permeation chromatography (gel permeation chromatography, GPC). Agilent HPLC-1260 high performance liquid chromatograph, preparing: eppendorf column incubator, shodex KF-801, 802, 802.5 and 803 gel permeation chromatography columns, differential detector, G7129A autosampler. The molecular weight of the resin was measured at a column temperature of 40℃using hexafluoroisopropanol as the mobile phase. The data were processed using chromatographic workstation cirrus software to obtain weight average molecular weight Mw and number average molecular weight distribution Mn.
(2) Adhesion: samples of the polyamide molding composition were tested by red ink to characterize the adhesion of the bracket plastic to hardware: and (3) soaking the LED support material and the electroplated hardware material into red ink through an in-mold injection molding LED reflecting cup, immersing pins with the red ink, placing, and observing whether the red ink permeates into the reflecting cup.
If the red ink does not permeate into the reflecting cup for 5min, judging the density and grade as grade A;
if the red ink does not permeate into the reflecting cup for 3min but permeates for 5min, judging the density and grade as grade B;
if the red ink does not permeate into the reflecting cup for 1min but permeates for 3min, judging the density and grade as grade C;
if the red ink permeates into the reflecting cup within 1min, judging the density and grade as grade D;
if the density and grade are D, the poor adhesion of the plastic and hardware is proved, and the risk of lamp bead failure is caused. On the contrary, if the density and the grades are A, B and C, the packaged lamp bead has excellent air tightness and good reliability.
(3) Whiteness: the contrast of the material is evaluated as characterized by the whiteness index of the material: a test piece having a length of 60mm, a width of 60mm and a thickness of 1mm was prepared by injection molding the polyamide molding composition. The whiteness is calculated using Color Eye 7000A Color difference meter measurement L, a, b values:
W H =100-[(100-L) 2 +a 2 +b 2 ] 1/2 。
(3) Reflectivity: a test piece having a length of 60mm, a width of 60mm and a thickness of 1mm was prepared by injection molding the polyamide molding composition. The reflectance of the test piece to 460nm wavelength light was measured using a Color Eye 7000A Color difference meter.
Table 1: examples 1 to 8 Polyamide moulding composition components (parts by weight) and test results
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | Example 8 | |
| PA 6T/MPDT resin | 60 | 60 | 60 | 60 | 60 | 60 | 60 | 60 |
| Wollastonite A | 30 | 40 | 50 | 55 | 60 | 40 | 40 | 40 |
| Toner A | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 1.0 | 1.5 | 2.0 |
| Seal rating | B | B | A | A | A | B | B | B |
| Whiteness degree | 25.60 | 25.44 | 26.01 | 26.38 | 28.85 | 23.24 | 21.62 | 21.34 |
| Reflectance,% | 4.33 | 3.56 | 3.71 | 3.80 | 4.05 | 3.03 | 3.36 | 3.79 |
As is clear from examples 1 to 8, wollastonite of 40 to 55 parts and toner of 1.0 part gave a good effect, and a low value of 3.03% could be obtained by using PA 6T/MPDT resin as the resin matrix.
Table 2: examples 9 to 15 Polyamide moulding composition components (parts by weight) and test results
| Example 9 | Example 10 | Example 11 | Example 12 | Example 13 | Example 14 | Example 15 | |
| PA 6T/MPDT resin | 60 | 60 | 60 | 60 | 60 | 60 | 60 |
| Wollastonite A | 40 | 40 | 40 | 40 | |||
| Wollastonite B | 40 | ||||||
| Wollastonite C | 40 | ||||||
| Wollastonite D | 40 | ||||||
| Toner A | 1.0 | 1.0 | 1.0 | ||||
| Toner B | 1.0 | 1.5 | |||||
| Toner C | 1.0 | 1.5 | |||||
| Seal rating | B | B | B | A | B | B | B |
| Whiteness degree | 23.96 | 25.87 | 25.25 | 27.88 | 27.21 | 28.63 | 27.10 |
| Reflectance,% | 3.26 | 4.56 | 5.11 | 4.26 | 3.90 | 5.43 | 5.19 |
As is evident from examples 6/9/10/11, wollastonite preferably has an average diameter of 7 to 15. Mu.m, and an average length of 80 to 160. Mu.m.
As is evident from examples 6/12-15, the toner is preferably an unoriented carbon toner.
Table 3: examples 16 to 21 Polyamide moulding compositions components (parts by weight) and test results
| Example 16 | Example 17 | Example 18 | Example 19 | Example 20 | Example 21 | |
| PA6T resin | 60 | |||||
| PA6T/6T MPDT resin-1 | 60 | |||||
| PA6T/6T MPDT resin-2 | 60 | |||||
| PA6T/6T MPDT resin-3 | 60 | |||||
| PA6T/6T MPDT resin-4 | 60 | |||||
| PA6T/6T MPDT resin-5 | 60 | |||||
| Wollastonite A | 40 | 40 | 40 | 40 | 40 | 40 |
| Toner A | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
| Seal rating | B | B | A | A | B | B |
| Whiteness degree | 23.79 | 23.67 | 23.65 | 23.51 | 23.56 | 23.37 |
| Reflectance,% | 3.42 | 4.67 | 4.52 | 4.13 | 3.60 | 3.28 |
As is clear from examples 6/17-21, the PA6T/6T MPDT preferably has a 2-methyl-1, 5-pentanediamine content of 20 to 100mol%, more preferably 60 to 100mol%.
Table 4: examples 22 to 27 Polyamide moulding compositions components (parts by weight) and test results
| Example 22 | Example 23 | Example 24 | Example 25 | Example 26 | Example 27 | |
| PA6T/6 IMPDI resin-1 | 60 | 60 | 60 | |||
| PA6T/6 IMPDI resin-2 | 60 | |||||
| PA6T/6 IMPDI resin-3 | 60 | |||||
| PA6T/6 IMPDI resin-4 | 60 | |||||
| Wollastonite A | 40 | 40 | 40 | 40 | 30 | |
| Wollastonite B | 30 | |||||
| Toner A | 1.0 | 1.0 | 1.0 | 1.0 | 0.5 | |
| Toner B | 0.4 | |||||
| Seal rating | C | B | B | B | C | C |
| Whiteness degree | 24.01 | 23.55 | 23.60 | 23.42 | 25.84 | 29.25 |
| Reflectance,% | 5.06 | 4.66 | 4.18 | 3.75 | 6.34 | 7.38 |
As can be seen from examples 22-25, PA6T/6 IMPDI preferably has a 2-methyl-1, 5-pentanediamine content of 20-100 mole%, more preferably 60-100 mole%.
As is evident from examples 26-27, the present invention provides PA6T/X molding compositions with good adhesion to hardware by adding toner, wollastonite to adjust whiteness to less than 30 and reflectance to less than 8%.
Table 5: comparative examples 1 to 6 Polyamide moulding compositions components (parts by weight) and test results
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | |
| PA6T 6I resin | 60 | 60 | 60 | |||
| PA6T resin | 60 | |||||
| PA6T/6TMPDT resin-1 | 60 | |||||
| PA6T/6 IMPDI resin-1 | 60 | |||||
| Wollastonite A | 40 | 40 | 40 | 40 | 10 | |
| Talc powder | 40 | |||||
| Toner A | 0.1 | 0.1 | 0.1 | 0.1 | 0.5 | 0.5 |
| Seal rating | A | D | C | B | D | C |
| Whiteness degree | 36.76 | 35.53 | 36.48 | 36.76 | 26.31 | 25.20 |
| Reflectance,% | 9.28 | 8.49 | 9.56 | 10.68 | 9.28 | 10.07 |
Table 6: comparative examples 7 to 11 Polyamide moulding compositions components (parts by weight) and test results
| Comparative example 7 | Comparative example 8 | Comparative example 9 | Comparative example 10 | Comparative example 11 | |
| PA6T/6TMPDT resin-1 | 60 | 60 | 60 | ||
| PA 6T/6I MPDI resin-5 | 60 | ||||
| PA 6T/6I MPDI resin-6 | 60 | ||||
| Wollastonite A | 40 | 40 | |||
| Wollastonite B | 30 | 30 | |||
| Talc powder | 40 | ||||
| Toner A | 0.2 | 0.3 | 0.5 | ||
| Toner B | 0.4 | 0.4 | |||
| Seal rating | A | A | D | C | C |
| Whiteness degree | 35.38 | 31.60 | 26.24 | 30.36 | 29.07 |
| Reflectance,% | 9.04 | 7.87 | 8.85 | 8.01 | 8.19 |
Claims (11)
1. A polyamide molding composition is characterized by comprising the following components in parts by weight:
40-70 parts of PA6T/X resin;
30-60 parts of wollastonite;
0.4-5 parts of toner;
based on the mole percent of PA6T/X, the content of 6T units is 50-70mol percent, and the content of X units is 30-50mol percent;
wherein the X unit consists of a diacid unit and a diamine unit, the diacid unit comprises one or a combination of more of terephthalic acid unit and isophthalic acid unit, the diamine unit comprises 1, 6-hexamethylenediamine unit and/or 2-methyl-1, 5-pentanediamine unit, and the 2-methyl-1, 5-pentanediamine in the diamine unit accounts for 60-100mol percent based on the mole percent of the X unit;
wollastonite has an average diameter of 7 to 15 μm and an average length of 80 to 160 μm in the polyamide molding composition;
the whiteness of the polyamide molding composition is less than 30, and the light source reflectivity of 460nm is less than 8%.
2. The polyamide molding composition according to claim 1, wherein the wollastonite content is 40 to 55 parts.
3. The polyamide molding composition according to claim 1, wherein the 6T unit content is 50 to 60mol% and the X unit content is 40 to 50mol%, based on the PA6T/X mole percentage.
4. A polyamide molding composition as claimed in claim 3, wherein the diamine of the X unit in PA6T/X is 2-methyl-1, 5-pentanediamine.
5. A polyamide molding composition as claimed in claim 3, wherein the PA6T/X has a number average molecular weight in the range from 1000 to 30000.
6. The polyamide molding composition of claim 1 wherein said toner is selected from the group consisting of carbon black, and mixed color toners.
7. The polyamide molding composition of claim 6 wherein said toner is selected from the group consisting of non-oriented carbon toners.
8. The polyamide molding composition of claim 1, wherein the 460nm light source reflectance is less than 6%.
9. The polyamide molding composition of claim 8, wherein the 460nm light source has a reflectance of 3 to 5%.
10. The polyamide molding composition as claimed in claim 1, further comprising 0 to 3 parts by weight of an antioxidant; the antioxidant is at least one selected from hindered phenol antioxidants, hindered amine antioxidants, phosphite antioxidants, mercaptan antioxidants and thiodipropionate antioxidants.
11. Use of a polyamide moulding composition according to any of claims 1 to 9 for the preparation of a reflective support for LED light sources.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002284990A (en) * | 2001-03-28 | 2002-10-03 | Asahi Kasei Corp | Highly weather-resistant polyamide resin composition |
| JP2011178908A (en) * | 2010-03-02 | 2011-09-15 | Toray Ind Inc | Polyester film comprising non-halogen flame retardant |
| CN105504789A (en) * | 2014-10-10 | 2016-04-20 | Ems专利股份公司 | Reinforced polyamide moulding compositions and injection mouldings produced therefrom |
| CN105585841A (en) * | 2014-11-11 | 2016-05-18 | Ems专利股份公司 | Polyamide Moulding Compound, Moulded Article Produced Herefrom And Also Purposes Of Use |
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| ES2215058T3 (en) * | 1999-08-02 | 2004-10-01 | E.I. Du Pont De Nemours And Company | AROMATIC POLYAMIDE COMPOSITIONS FOR MOLDING. |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002284990A (en) * | 2001-03-28 | 2002-10-03 | Asahi Kasei Corp | Highly weather-resistant polyamide resin composition |
| JP2011178908A (en) * | 2010-03-02 | 2011-09-15 | Toray Ind Inc | Polyester film comprising non-halogen flame retardant |
| CN105504789A (en) * | 2014-10-10 | 2016-04-20 | Ems专利股份公司 | Reinforced polyamide moulding compositions and injection mouldings produced therefrom |
| CN105585841A (en) * | 2014-11-11 | 2016-05-18 | Ems专利股份公司 | Polyamide Moulding Compound, Moulded Article Produced Herefrom And Also Purposes Of Use |
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