CN114656781A - Gray semi-aromatic polyamide molding material and preparation method and application thereof - Google Patents
Gray semi-aromatic polyamide molding material and preparation method and application thereof Download PDFInfo
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Abstract
A grey semi-aromatic polyamide molding material comprises the following components in parts by weight: 40-75 parts of PA10T/X resin; 30-60 parts of wollastonite; 0.5-2.5 parts of toner; 5-35 parts of a white pigment; the wollastonite has an average diameter of 4 to 20 micrometers and an average length of 40 to 250 micrometers, and the white pigment has an average particle size of 0.10 to 0.50 micrometer; the grey semi-aromatic polyamide molding material is subjected to differential scanning calorimetry, and the full width at half maximum of a crystallization peak Delta T is measured at the cooling rate of 20 ℃/min after the temperature is raised to 345 DEG C1/2Is 3.5 to 11 ℃; the gray semi-aromatic polyamide molding materialThe whiteness range of the material is 50-80, the reflectance range of a purple light (400 nm wavelength) light source is 16-36%, the reflectance range of a blue light (460 nm wavelength) light source is 22-49%, and the reflectance of a red light (650 nm wavelength) light source is lower than that of the blue light by more than 1%. The molding materials of the invention have the combined properties of low violet reflectance in grey, high brightness (high blue reflectance) and high contrast (red reflectance lower than blue reflectance).
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a gray semi-aromatic polyamide molding material and a preparation method and application thereof.
Background
The LED light source mainly comprises a semiconductor chip, an LED light source reflection bracket, a gold wire and packaging glue. The LED light source reflection support is a framework of the LED light source and is also a functional part. In the LED packaging process, other materials and components are integrated through die bonding, wire bonding and packaging adhesive curing. The LED reflection bracket needs to reflect light emitted from the LED chip through a certain angle, so as to reduce light loss, and then the light passes through the epoxy resin or the silica gel and other packaging materials, so as to form a light source for LED illumination or display. The LED reflecting bracket material is a core material of LED illumination and is directly related to the performance and the service life of an LED light source.
At present, when selecting the material of the LED reflection support, in addition to the characteristics of encapsulation, fluidity, weather resistance, etc., the reflectivity of the LED reflection support needs to be considered:
in the application field of LED display, the brightness and contrast of the display screen are very important indexes for displaying the sharpness of the image quality. The LED support mainly used in the current market is produced by pure white LED reflecting materials, black ink is needed to be silk-screened on the surface of the LED support, the process is complicated, the efficiency is influenced, the cost is high, the side surface and the surface of the reflecting cup are still white, and the contrast and the gray scale displayed by an LED display screen are reduced. However, in the field of outdoor display, higher brightness is often required, so the prior art mainly uses silver plating on the bottom of the cup of the LED bracket to improve the reflectivity or increase the light quantity of the light source. But this increases the cost. If the LED reflector bracket is white, the contrast is low.
With respect to the light source: the LED full-color display screen light source is formed by packaging three chips, namely red (R), green (G) and blue (B), wherein the luminous brightness of the blue light chip is lowest, namely, the contrast is highest, so that the LED light source support can directly influence the overall contrast of the LED display screen on the blue light reflectivity of the used chip. In order to improve the brightness and the contrast of the outdoor LED display screen, it is a better method to increase the reflectivity of blue light so that the brightness of the blue light is as larger as possible than that of red light.
Disclosure of Invention
The invention aims to overcome the technical defects and provide a gray semi-aromatic polyamide molding material which realizes high contrast and high reflectivity under gray tone so as to achieve the effect of simultaneously combining the contrast, the gray level and the brightness of an LED display screen.
The invention is realized by the following technical scheme:
a grey semi-aromatic polyamide molding material comprises the following components in parts by weight:
40-75 parts of PA10T/X resin;
30-60 parts of wollastonite;
0.5-2.5 parts of toner;
5-35 parts of a white pigment;
based on mole percent PA10T/X, the content of 10T units is 60-100mol%, and the content of X units is 0-40 mol%; wherein the unit X is composed of diacid unit and diamine unit, the diacid unit is selected from at least one of terephthalic acid unit, isophthalic acid unit, 1, 6-adipic acid and 1, 10-sebacic acid unit, the diamine unit is selected from at least one of 1, 6-hexanediamine unit, 1, 9-nonanediamine unit, 2-methyl-1, 5-pentanediamine unit, 2-methyl-1, 8-octanediamine unit, 1, 10-decanediamine unit and 1, 12-dodecanediamine unit;
the wollastonite has an average diameter of 4 to 20 micrometers and an average length of 40 to 250 micrometers, and the white pigment has an average particle size of 0.10 to 0.50 micrometer;
the grey semi-aromatic polyamide molding material is subjected to differential scanning calorimetry, and the full width at half maximum of a crystallization peak Delta T is measured at the cooling rate of 20 ℃/min after the temperature is raised to 345 DEG C1/2Is 3.5-11 ℃;
the whiteness range of the gray semi-aromatic polyamide molding material is 50-80, the reflectance range of a 400nm wavelength purple light source is 16-36%, the reflectance range of a 460nm wavelength blue light source is 22-49%, and the reflectance of a 650nm wavelength red light source is lower than that of a 460nm wavelength blue light source by more than 1%.
The semiaromatic polyamide molding materials exhibit a grey coloration in the whiteness range from 50 to 80.
The PA10T/X resin is selected from at least one of PA10T, PA10T/10I, PA10T/6T, PA10T/66, PA10T/1010, PA10T/610, PA10T/612 and PA 10T/12T.
Preferably, the semi-aromatic polyamide molding composite material is prepared by differential scanning calorimetry, and the full width at half maximum of a crystallization peak Delta T measured at the cooling rate of 20 ℃/min after the temperature is raised to 345 DEG C1/2Is 4.5-8 ℃. The preferred semi-aromatic polyamide molding composite material with the half height width of the crystallization peak has larger difference of the reflectivity of a red light source with the wavelength of 650nm and the reflectivity of blue light.
The PA10T/X resin of the present invention may be a commercially available product or may be synthesized by the following method. For more precise experiments, the PA10T/X adopted in the examples and the comparative examples is a self-made sample, and the raw materials such as the reaction monomers, the end-capping reagent and the like are sourced from commercial products.
(1) Pre-polymerization: putting polymerization reaction monomers (diacid and diamine), an end-capping agent benzoic acid and deionization into a stainless steel high-pressure reaction kettle with mechanical stirringAnd (3) water. Vacuuming and using N2After the third replacement, the temperature is raised and stirred, the temperature is raised to 190 ℃ at the temperature raising rate of 4-6 ℃/min, the temperature is kept constant for 1-2 hours, and then the temperature is raised to 280 ℃ at the temperature raising rate of 1-3 ℃/min, the temperature is slowly stirred and kept constant for 3-5 hours, so that the prepolymerization reaction is fully carried out. After the constant temperature is finished, the temperature is slowly raised to 270-290 ℃, and the water is drained to the normal pressure. And when the pressure is reduced to the normal pressure, closing a drain valve, finishing the reaction, and reducing the temperature to the room temperature for discharging.
(2) Solid-phase tackifying: and putting the materials prepared in the prepolymerization process into a vacuum rotary drum, wherein the rotating speed of the rotary drum is set to be 10-15 r/min, and the vacuum degree is set to be 25-35 Pa. Heating at a rate of 15-25 deg.C/min, sampling when the temperature reaches 260 deg.C and 270 deg.C, testing viscosity, and determining the discharge end point according to the viscosity (or number average molecular weight) result.
The number average molecular weight of the PA10T/X resin is 1500-28000.
The number average molecular weight test method is a conventional method, and specifically comprises the following steps: the number average molecular weight (Mn) of the PA10T/X resin samples was determined by Gel Permeation Chromatography (GPC). An Agilent HPLC-1260 high performance liquid chromatograph, which is prepared: eppendorf column incubators, Shodex KF-801, 802, 802.5 and 803 gel permeation chromatography columns, differential detector, G7129A autosampler. Hexafluoroisopropanol was used as a mobile phase, and the molecular weight of the resin was measured at a column temperature of 40 ℃. And processing the data by using cirrus software of a chromatographic workstation to obtain the number average molecular weight Mn.
The white pigment is at least one of titanium dioxide and zinc sulfide.
From the standpoint of increasing the difference between the reflectance of blue light and the reflectance of red light, it is preferred that the wollastonite have an average diameter of 6 to 13 μm, an average length of 80 to 120. mu.m, and the white pigment have an average particle diameter in the range of 0.15 to 0.35. mu.m. Wollastonite belongs to powder with a certain length-diameter ratio, the microstructure is fibrous, and the length and the diameter of the wollastonite are almost unchanged in the melting and shearing process in a screw. Experiments show that PA10T and wollastonite (with the average diameter of 17 μm and the average length of 180 μm) are subjected to melt shear blending through a production process, and the wollastonite is tested for the average diameter and the average length by using a solvent-dissolved resin, and the wollastonite is almost unchanged in diameter and changed in average length by about 0.5% in the shearing of a screw.
The toner is at least one or more of carbon black, black and amorphous carbon toner.
Preferably, the reflectance of the 650nm wavelength red light source is more than 2% lower than that of the 460nm wavelength blue light source.
The grey semi-aromatic polyamide moulding materials according to the invention may also comprise auxiliaries such as lubricants, antioxidants and the like.
The preparation method of the gray semi-aromatic polyamide molding material comprises the following steps of adding the components into a mixer for uniform mixing, and extruding and granulating through a double-screw extruder to obtain the gray semi-aromatic polyamide molding material; wherein the temperature range of the screw is 280-330 ℃ and the rotating speed is 400-500 r/min.
The gray semi-aromatic polyamide molding material is applied to preparing a light source reflecting bracket of an LED display screen, and particularly relates to an outdoor light source reflecting bracket of the LED display screen.
The invention has the following beneficial effects:
the reflectivity of the light source of the LED display screen is mainly related to the whiteness (L value) of the material (the lower the whiteness, the lower the reflectivity of the 400nm ultraviolet light), but is also influenced by the surface roughness of the material (the larger the roughness of the object surface is within a certain range, the more diffuse reflection occurs on the object surface by the light emitted from the light source, and the less light energy is finally received at the light receiving end). The influence of the LED display screen light source reflection support on the brightness, the gray scale and the contrast of the LED display screen mainly lies in the whiteness and the reflectivity of the light source reflection support. In order to realize good balance of brightness, gray scale and contrast of an outdoor display screen, the invention is mainly realized by the following scheme:
firstly, through blending of white pigment and toner, a color tone product with the whiteness of 50-80 can be obtained, and the product has higher light source reflectivity compared with a product with the whiteness of less than 30; and the negative impact of grey tones on grey scale and contrast can be controlled within acceptable limits compared to white products.
Secondly, by exploring the length/diameter of wollastonite, the particle size range of white pigment and the full width at half maximum of a crystallization peak of the gray semi-aromatic polyamide molding material, the reflectivity of a 460nm light source can be improved to a certain extent, so that the reflectivity of blue light is higher than that of red light, and the brightness and contrast of a display screen are improved.
Specifically, in the technical scheme of the invention, the half width at half maximum of the crystallization peak of the gray semi-aromatic polyamide molding material is mainly adjusted by adjusting the addition amounts and specifications of the toner, wollastonite and white pigment, and can also be obtained by selecting PA10T/X with different specifications.
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 invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The raw materials used in the examples and comparative examples are as follows:
the following monomers used for the polymerization of polyamides are commercially available products, pure for polymerization.
PA 10T: number average molecular weight of 7300, full width at half maximum of crystallization peak DeltaT1/2At 5 ℃, the product is self-made according to the method of the invention;
PA 10T/1010-1: 10T unit content 80mol%, number average molecular weight 7500, and half-height width of crystal peak DeltaT1/2The temperature is 15.1 ℃, and the method is self-made according to the method of the invention;
PA 10T/1010-2: 85mol% of 10T unit content, 9000 number average molecular weight, and Δ T of half height width of crystal peak1/2At 16 ℃, self-made according to the method in the invention;
PA 10T/1010-3: 90mol% of 10T unit content, number average molecular weight 8500, and half-height width of crystallization peak DeltaT1/2The temperature is 12.8 ℃, and the method is self-made according to the method of the invention;
PA 10T/1010-4: 95mol% of 10T unit content, 13000 number average molecular weight, and Delta T of full width at half maximum of crystallization peak1/2The temperature is 8.4 ℃, and the method is self-made according to the method of the invention;
PA 10T/1010-5: 90mol% of 10T unit content, 4300 number average molecular weight, and Δ T of full width at half maximum of crystallization peak1/2At 14.2 ℃, the product is self-made according to the method of the invention;
PA 10T/1010-6: 90mol% of 10T unit content, number average molecular weight of 21000, and half-height width of crystallization peak Delta T1/2At 18.3 ℃, the product is self-made according to the method of the invention;
PA 10T/1010-7: 75mol% of 10T unit content, number average molecular weight 8800, half height width of crystallization peak DeltaT1/2At 18.0 ℃, the product is self-made according to the method of the invention;
PA 10T/1010-8: 97mol% of 10T unit content, 8000 number average molecular weight, half height width of crystallization peak delta T1/2At 7.5 ℃, the product is self-made according to the method of the invention;
PA 10T/10I-1: the content of 10T unit is 80mol%, the number average molecular weight is 10500, and the full width at half maximum of crystallization peak is delta T1/2At the temperature of 17.1 ℃, the product is self-made according to the method of the invention;
PA 10T/10I-2: 85mol% of 10T unit content, 9800 of number average molecular weight and delta T of full width at half maximum of crystallization peak1/2At 12 ℃, the product is self-made according to the method of the invention;
PA 10T/10I-3: 90mol% of 10T unit content, number average molecular weight 8500, and half-height width of crystallization peak DeltaT1/2The temperature is 8.3 ℃, and the method is self-made according to the method of the invention;
PA 10T/10I-4: 95mol% of 10T unit content, 8000 number average molecular weight, half height width of crystallization peak delta T1/2At 7.1 ℃, the product is self-made according to the method of the invention;
PA 10T/10I-5: 60mol% of 10T unit content, 8000 number average molecular weight, half height width of crystallization peak delta T1/2At 15 ℃, the product is self-made according to the method of the invention;
PA 10T/66: the content of 10T unit is 90mol%, the number average molecular weight is 8000, and the half-height width Delta T of crystallization peak1/2The temperature is 13.4 ℃, and the method is self-made according to the method in the invention;
wollastonite A: average diameter of 4 microns and average length of 60 microns;
wollastonite B: average diameter of 6 microns and average length of 120 microns;
wollastonite C: average diameter of 13 microns and average length of 80 microns;
wollastonite D: the average diameter was 19 microns and the average length was 230 microns.
The wollastonite used in the present invention is commercially available and then screened to obtain the desired average diameter and average length range.
Talc powder: AH-1250, Guangxi Longsheng Huamei Talc development Co.
Titanium dioxide A: average particle size 0.11 microns;
titanium dioxide B: average particle size 0.15 microns;
titanium dioxide C: average particle size 0.35 microns;
titanium dioxide D: average particle size 0.50 microns;
the titanium dioxide is purchased from the dragon boa herboria, and samples with corresponding particle sizes are obtained by screening.
Zinc sulfide: sachtolith HD-S, average particle size 0.14 microns, available from Shaharley, Germany.
Toner a: amorphous carbon toner N774, tianjin tianyang autumn actualization industrial technology ltd;
toner B: carbon black M570, cabot chemical limited;
toner C: black UN2014, cabot chemical limited;
toner D: mazcol Blue 153K, Shenzhen Shentai chemical Co.
Antioxidant: commercially available, parallel experiments were performed with the same antioxidant.
Examples and comparative examples the preparation of grey semi-aromatic polyamide moulding materials: adding PA10T/X resin, wollastonite, toner and white pigment into a mixer, uniformly mixing, and extruding and granulating by a double-screw extruder to obtain a gray semi-aromatic polyamide molding material; wherein the temperature range of the screw is 280 ℃ and 330 ℃, and the rotating speed is 450 r/min.
The test method comprises the following steps:
(1) whiteness: the contrast of the evaluated materials is characterized by the whiteness index of the material: test pieces having a length of 60mm, a width of 60mm and a thickness of 1mm prepared by injection molding a gray semi-aromatic polyamide molding material were measured for the whiteness using a Color Eye 7000A type Color difference meter:
WH=100-[(100-L)2+a2+b2]1/2。
(2) reflectance ratio: a gray semi-aromatic polyamide molding material was injection-molded to prepare a test piece having a length of 60mm, a width of 60mm and a thickness of 1 mm. The reflectance of the test piece at wavelengths of 400nm, 460nm and 650nm was measured using a Color Eye 7000A colorimeter.
(3) Half-height width of crystalline peak Delta T of gray semi-aromatic polyamide molding material1/2: heating to 345 deg.C at 20 deg.C/min from 30 deg.C in nitrogen atmosphere by using Differential Scanning Calorimetry (DSC) manufactured by NETZSCH, maintaining the temperature for 2min, cooling at 20 deg.C/min, setting the temperature of the crystallization peak at the temperature of Tc (deg.C), and determining half temperature of the peak width as the half height width of the crystallization peak Δ T1/2。
Table 1: examples 1 to 7 Gray semi-aromatic Polyamide moulding Material Components (parts by weight) and test results
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | |
| PA10T | 75 | 70 | 65 | 60 | 55 | 50 | 40 |
| Wollastonite A | 30 | 35 | 40 | 45 | 50 | 55 | 60 |
| Titanium white powder A | 35 | 25 | 20 | 20 | 20 | 15 | 5 |
| Toner A | 2.5 | 2 | 1.5 | 1 | 1 | 1 | 0.5 |
| Full width at half maximum of crystalline peak Δ T1/2，℃ | 3.5 | 3.8 | 4 | 4.3 | 4.5 | 4.6 | 4.8 |
| Whiteness degree | 50.4 | 51.5 | 53.5 | 57.3 | 64.1 | 69.1 | 74.0 |
| Reflectance at a wavelength of 400 nm% | 16.48 | 18.37 | 20.26 | 22.57 | 26.66 | 30.7 | 35.74 |
| 460nm wavelength reflectance% | 22.12 | 23.93 | 24.73 | 27.5 | 34.26 | 41.17 | 48.09 |
| Reflectance at 460nm wavelength and reflectance at 650nm wavelengthDifference in refractive index% | 1.80 | 1.95 | 1.08 | 1.80 | 2.25 | 2.26 | 2.29 |
From examples 1 to 7, it can be seen that the content of the components of the formulation significantly affects the full width at half maximum of the crystallization peak and the whiteness of the molding materials, and that within the scope of the invention, a reflectance range of 16 to 36% for a violet light source with a wavelength of 400nm, a reflectance range of 22 to 49% for a blue light source with a wavelength of 460nm and a reflectance of more than 1% for a red light source with a wavelength of 650nm can be achieved.
Table 2: examples 8 to 14 compositions (in parts by weight) of grey semi-aromatic polyamide moulding materials and test results
| Example 8 | Example 9 | Example 10 | Example 11 | Example 12 | Example 13 | Example 14 | |
| PA10T/1010-1 | 60 | ||||||
| PA10T/1010-2 | 60 | ||||||
| PA10T/1010-3 | 60 | ||||||
| PA10T/1010-4 | 60 | ||||||
| PA10T/1010-5 | 60 | ||||||
| PA10T/1010-6 | 60 | ||||||
| PA10T/1010-7 | 60 | ||||||
| Wollastonite A | 45 | 45 | 45 | 45 | 45 | 45 | 45 |
| Titanium white powder A | 20 | 20 | 20 | 20 | 20 | 20 | 20 |
| Toner A | 1 | 1 | 1 | 1 | 1 | 1 | 1 |
| Full width at half maximum of crystalline peak Δ T1/2，℃ | 8.3 | 9.0 | 6.9 | 5.1 | 8.5 | 10.3 | 9.7 |
| Whiteness degree | 57.2 | 58.0 | 57.6 | 57.0 | 57.5 | 56.9 | 57.4 |
| Reflectance at a wavelength of 400 nm% | 22.75 | 23.01 | 22.84 | 22.90 | 23.11 | 22.50 | 22.81 |
| 460nm wavelength reflectance% | 27.53 | 27.72 | 27.49 | 27.70 | 28.04 | 27.88 | 27.46 |
| The difference between the 460nm wavelength reflectance and the 650nm wavelength reflectance% | 1.75 | 1.66 | 2.04 | 2.19 | 1.89 | 1.54 | 1.92 |
From examples 4/8-21, it is clear that the half height width of the peak of crystallization of the gray semi-aromatic polyamide molding material obtained by compounding wollastonite, a white pigment and a toner is within a range of 3.5 to 11 ℃, and further that when the half height width of the peak of crystallization is within a range of 4.5 to 8 ℃, the difference between the reflectance at 460nm wavelength and the reflectance at 650nm wavelength is more than 2%.
Table 3: examples 15 to 21 parts by weight of Gray semiaromatic Polyamide moulding Material and test results
| Example 15 | Example 16 | Example 17 | Example 18 | Example 19 | Example 20 | Example 21 | |
| PA10T/1010-8 | 60 | ||||||
| PA10T/10I-1 | 60 | ||||||
| PA10T/10I-2 | 60 | ||||||
| PA10T/10I-3 | 60 | ||||||
| PA10T/10I-4 | 60 | ||||||
| PA10T/10I-5 | 60 | ||||||
| PA10T/66 | 60 | ||||||
| Wollastonite A | 45 | 45 | 45 | 45 | 45 | 45 | 45 |
| Titanium white powder A | 20 | 20 | 20 | 20 | 20 | 20 | 20 |
| Toner A | 1 | 1 | 1 | 1 | 1 | 1 | 1 |
| Full width at half maximum of crystalline peak Δ T1/2，℃ | 4.9 | 9.6 | 6.4 | 4.9 | 4.2 | 8.2 | 6.3 |
| Whiteness degree | 56.9 | 58.1 | 57.5 | 57.7 | 57.2 | 56.7 | 57.1 |
| Reflectance at a wavelength of 400 nm% | 22.25 | 23.20 | 23.16 | 22.84 | 23.05 | 23.32 | 22.50 |
| 460nm wavelength reflectance% | 27.38 | 28.06 | 28.34 | 28.55 | 28.61 | 28.03 | 27.81 |
| The difference between the 460nm wavelength reflectance and the 650nm wavelength reflectance% | 2.30 | 1.84 | 2.51 | 2.15 | 1.99 | 1.54 | 2.36 |
Table 4: examples 22 to 27 Gray semi-aromatic Polyamide moulding Material Components (parts by weight) and test results
| Example 22 | Example 23 | Example 24 | Example 25 | Example 26 | Example 27 | |
| PA10T | 60 | 60 | 60 | 60 | 60 | 60 |
| Wollastonite A | 45 | 45 | ||||
| Wollastonite B | 45 | |||||
| Wollastonite C | 45 | |||||
| Wollastonite D | 45 | 45 | ||||
| Titanium white powder A | 20 | |||||
| Titanium white B | 20 | 20 | ||||
| Titanium white powder C | 20 | 20 | ||||
| Titanium dioxide D | 20 | |||||
| Toner A | 1 | 1 | 1 | 1 | 1 | 1 |
| Full width at half maximum of crystalline peak Δ T1/2，℃ | 4.2 | 4.5 | 4.6 | 4.4 | 4.2 | 4.3 |
| Whiteness degree | 57.9 | 57.5 | 56.9 | 57.2 | 57.4 | 56.9 |
| Reflectance at a wavelength of 400 nm% | 22.72 | 22.83 | 23.00 | 23.16 | 23.42 | 22.84 |
| 460nm wavelength reflectance% | 27.90 | 28.10 | 28.41 | 28.06 | 28.80 | 27.87 |
| The difference between the reflectance at a wavelength of 460nm and the reflectance at a wavelength of 650 nm% | 2.35 | 2.84 | 2.08 | 1.85 | 1.86 | 1.66 |
It is known from 4/22-27 that the particle size of wollastonite and titanium dioxide also affects the half height width of the crystallization peak of the gray semi-aromatic polyamide molding material, and the particle size range of the preferred wollastonite and titanium dioxide can further increase the difference between the 460nm wavelength reflectance and the 650nm wavelength reflectance, and when the half height width of the crystallization peak of the gray semi-aromatic polyamide molding material is at 4.5 ℃, the difference between the 460nm wavelength reflectance and the 650nm wavelength reflectance is further increased.
Table 5: examples 28 to 31 Components (parts by weight) of Gray semi-aromatic Polyamide moulding materials and test results
| Example 28 | Example 29 | Example 30 | Example 31 | |
| PA10T | 60 | 60 | 60 | 60 |
| Wollastonite A | 45 | 45 | 45 | 45 |
| Titanium white powder A | 20 | 20 | 20 | |
| Zinc sulphide | 20 | |||
| Toner A | 0.5 | 1 | ||
| Toner B | 1 | |||
| Toner C | 1 | |||
| Toner D | 0.5 | |||
| Full width at half maximum of crystalline peak Δ T1/2，℃ | 4.1 | 4.3 | 4.4 | 4.1 |
| Whiteness degree | 58.15 | 57.34 | 59.90 | 55.66 |
| Reflectance at a wavelength of 400 nm% | 23.04 | 22.72 | 23.63 | 22.53 |
| 460nm wavelength reflectance% | 28.27 | 28.05 | 28.61 | 27.77 |
| The difference between the reflectance at a wavelength of 460nm and the reflectance at a wavelength of 650 nm% | 1.54 | 1.83 | 1.77 | 1.51 |
From examples 4/28-31, it can be seen that the reflectance of zinc sulfide is lower than that of titanium dioxide.
Table 6: comparative example component (parts by weight) of Gray semi-aromatic Polyamide moulding Material and test results
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | |
| PA10T | 60 | 60 | 60 | 40 | |
| PA10T/1010-6 | 60 | ||||
| Wollastonite A | 45 | 45 | 45 | 45 | |
| Talcum powder | 45 | ||||
| Titanium white powder A | 20 | 5 | 20 | 10 | 35 |
| Toner A | 0.2 | 2.5 | 1 | 0.5 | 3.0 |
| Full width at half maximum of crystalline peak Δ T1/2，℃ | 4.7 | 3.6 | 4.1 | 11.1 | 3.2 |
| Whiteness degree | 97.14 | 43 | 58.15 | 69.12 | 46.75 |
| Reflectance at a wavelength of 400 nm% | 46.62 | 12.28 | 23.04 | 29.7 | 16.07 |
| 460nm wavelength reflectance% | 93.6 | 13.12 | 28.27 | 41.17 | 16.16 |
| The difference between the reflectance at a wavelength of 460nm and the reflectance at a wavelength of 650 nm% | -0.88 | 0.16 | 0.24 | 0.47 | 0.84 |
As can be seen from comparative example 1, when the whiteness is too high, the reflectance of red light is higher than that of blue light.
As can be seen from comparative example 2, when the whiteness is too low, the reflectance of each spectrum is low, and the difference in reflectance of blue light and red light is also small.
As can be seen from comparative example 3, when talc was used as a filler in place of wollastonite, the difference in reflectance between blue light and red light was small.
From comparative examples 4 and 5, it can be seen that the difference in the reflectance of blue light and red light is also small when the half width of the crystalline peak of the gray semi-aromatic polyamide molding material is outside the range of 3.5 to 11 ℃.
Claims (10)
1. A grey semi-aromatic polyamide molding material is characterized by comprising the following components in parts by weight:
40-75 parts of PA10T/X resin;
30-60 parts of wollastonite;
0.5-2.5 parts of toner;
5-35 parts of a white pigment;
based on mole percent PA10T/X, the content of 10T units is 60-100mol%, and the content of X units is 0-40 mol%; wherein the unit X is composed of diacid unit and diamine unit, the diacid unit is selected from at least one of terephthalic acid unit, isophthalic acid unit, 1, 6-adipic acid and 1, 10-sebacic acid unit, the diamine unit is selected from at least one of 1, 6-hexanediamine unit, 1, 9-nonanediamine unit, 2-methyl-1, 5-pentanediamine unit, 2-methyl-1, 8-octanediamine unit, 1, 10-decanediamine unit and 1, 12-dodecanediamine unit;
the wollastonite has an average diameter of 4 to 20 micrometers and an average length of 40 to 250 micrometers, and the white pigment has an average particle size of 0.10 to 0.50 micrometer;
the grey semi-aromatic polyamide molding material is subjected to differential scanning calorimetry, and the full width at half maximum of a crystallization peak Delta T is measured at the cooling rate of 20 ℃/min after the temperature is raised to 345 DEG C1/2Is 3.5-11 ℃;
the whiteness range of the gray semi-aromatic polyamide molding material is 50-80, the reflectance range of a 400nm wavelength purple light source is 16-36%, the reflectance range of a 460nm wavelength blue light source is 22-49%, and the reflectance of a 650nm wavelength red light source is lower than that of a 460nm wavelength blue light source by more than 1%.
2. A grey semi-aromatic polyamide moulding material according to claim 1, characterized in that the PA10T/X resin is selected from at least one of PA10T, PA10T/10I, PA10T/6T, PA10T/66, PA10T/1010, PA10T/610, PA10T/612 and PA 10T/12T.
3. A grey semi-aromatic polyamide moulding material according to claim 1, characterised in that the semi-aromatic polyamide moulding composite is characterised by a half-height width at half maximum Δ T of the crystallisation peak measured by differential scanning calorimetry at a cooling rate of 20 ℃/min after having been heated to 345 ℃1/2Is 4.5-8 ℃.
4. A grey semi-aromatic polyamide moulding material as claimed in claim 1, characterized in that the PA10T/X resin has a number average molecular weight of 1500-28000.
5. A grey semi-aromatic polyamide moulding material according to claim 1, characterized in that the white pigment is selected from at least one of titanium dioxide and zinc sulphide.
6. A gray semi-aromatic polyamide molding material as claimed in claim 1, characterized in that the wollastonite has an average diameter of 6 to 13 μm and an average length of 80 to 120 μm and the white pigment has an average particle diameter in the range from 0.15 to 0.35. mu.m.
7. A grey semi-aromatic polyamide moulding material according to claim 1, characterised in that the toner is at least one or more colour-blending toners selected from carbon black, black and amorphous carbon toners.
8. A grey semi-aromatic polyamide moulding material according to claim 1, characterised in that the reflectance of a 650nm wavelength red light source is more than 2% lower than the reflectance of a 460nm wavelength blue light source.
9. A process for the preparation of a grey semi-aromatic polyamide moulding material according to any of claims 1 to 10, characterised in that it comprises the steps of adding the components to a compounder and mixing them homogeneously, followed by extrusion granulation through a twin-screw extruder to obtain a grey semi-aromatic polyamide moulding material; wherein the temperature range of the screw is 280-330 ℃, and the rotation speed is 400-500 r/min.
10. Use of a grey semi-aromatic polyamide moulding material according to any of claims 1 to 9 for the production of LED display screen light source reflective supports.
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