WO2023040943A1 - 一种聚酰胺模塑复合材料及其制备方法和应用 - Google Patents
一种聚酰胺模塑复合材料及其制备方法和应用 Download PDFInfo
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- WO2023040943A1 WO2023040943A1 PCT/CN2022/118970 CN2022118970W WO2023040943A1 WO 2023040943 A1 WO2023040943 A1 WO 2023040943A1 CN 2022118970 W CN2022118970 W CN 2022118970W WO 2023040943 A1 WO2023040943 A1 WO 2023040943A1
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- WIPO (PCT)
- Prior art keywords
- semi
- aromatic polyamide
- polyamide molding
- pa10t
- unit
- Prior art date
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- 238000000465 moulding Methods 0.000 title claims abstract description 55
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims description 5
- 239000004952 Polyamide Substances 0.000 title description 4
- 229920002647 polyamide Polymers 0.000 title description 4
- 229920006012 semi-aromatic polyamide Polymers 0.000 claims abstract description 51
- 238000002425 crystallisation Methods 0.000 claims abstract description 32
- 230000008025 crystallization Effects 0.000 claims abstract description 32
- 229920005989 resin Polymers 0.000 claims abstract description 15
- 239000011347 resin Substances 0.000 claims abstract description 15
- 229920006119 nylon 10T Polymers 0.000 claims description 58
- 239000010456 wollastonite Substances 0.000 claims description 36
- 229910052882 wollastonite Inorganic materials 0.000 claims description 36
- 150000001875 compounds Chemical class 0.000 claims description 26
- 239000003963 antioxidant agent Substances 0.000 claims description 9
- 229910003481 amorphous carbon Inorganic materials 0.000 claims description 6
- 230000003078 antioxidant effect Effects 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000011159 matrix material Substances 0.000 claims description 5
- 125000004427 diamine group Chemical group 0.000 claims description 4
- 238000000113 differential scanning calorimetry Methods 0.000 claims description 4
- 239000000805 composite resin Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- GAGWMWLBYJPFDD-UHFFFAOYSA-N 2-methyloctane-1,8-diamine Chemical group NCC(C)CCCCCCN GAGWMWLBYJPFDD-UHFFFAOYSA-N 0.000 claims description 2
- JZUHIOJYCPIVLQ-UHFFFAOYSA-N 2-methylpentane-1,5-diamine Chemical group NCC(C)CCCN JZUHIOJYCPIVLQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000001361 adipic acid Substances 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- YQLZOAVZWJBZSY-UHFFFAOYSA-N decane-1,10-diamine Chemical group NCCCCCCCCCCN YQLZOAVZWJBZSY-UHFFFAOYSA-N 0.000 claims description 2
- 125000001142 dicarboxylic acid group Chemical group 0.000 claims description 2
- QFTYSVGGYOXFRQ-UHFFFAOYSA-N dodecane-1,12-diamine Chemical group NCCCCCCCCCCCCN QFTYSVGGYOXFRQ-UHFFFAOYSA-N 0.000 claims description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical group NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical group OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 2
- SXJVFQLYZSNZBT-UHFFFAOYSA-N nonane-1,9-diamine Chemical group NCCCCCCCCCN SXJVFQLYZSNZBT-UHFFFAOYSA-N 0.000 claims description 2
- 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 2
- 239000004760 aramid Substances 0.000 claims 1
- 229920003235 aromatic polyamide Polymers 0.000 claims 1
- 238000005453 pelletization Methods 0.000 claims 1
- 238000002310 reflectometry Methods 0.000 abstract description 19
- 238000012858 packaging process Methods 0.000 abstract description 4
- 230000007774 longterm Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 18
- 239000000463 material Substances 0.000 description 17
- 238000012360 testing method Methods 0.000 description 13
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- 239000011324 bead Substances 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 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
- 238000002474 experimental method Methods 0.000 description 3
- 238000005227 gel permeation chromatography Methods 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000010998 test method Methods 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
- ODJQKYXPKWQWNK-UHFFFAOYSA-L 3-(2-carboxylatoethylsulfanyl)propanoate Chemical compound [O-]C(=O)CCSCCC([O-])=O ODJQKYXPKWQWNK-UHFFFAOYSA-L 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000011156 evaluation Methods 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
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012299 nitrogen atmosphere 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
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 210000001525 retina Anatomy 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
- 108700012359 toxins Proteins 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/12—Making granules characterised by structure or composition
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
- B29B7/06—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices
- B29B7/10—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary
- B29B7/18—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with more than one shaft
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
- B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
- B29B7/46—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
- B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
- B29B7/46—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft
- B29B7/48—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft with intermeshing devices, e.g. screws
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/10—Making granules by moulding the material, i.e. treating it in the molten state
-
- 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
-
- 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
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2077/00—Use of PA, i.e. polyamides, e.g. polyesteramides or derivatives thereof, as moulding material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
- B29K2105/06—Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/265—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids from at least two different diamines or at least two different dicarboxylic acids
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
Definitions
- the invention relates to the technical field of polymer materials, in particular to a polyamide molding composite material and its preparation method and application.
- the LED light source is mainly composed of semiconductor chips, LED light source reflection brackets, gold wires, and packaging glue.
- the LED light source reflector bracket is the "skeleton" of the LED light source, and it is also a functional part.
- the LED packaging process needs to go through crystal bonding, wire bonding, and packaging glue curing, and other materials and components are integrated here.
- the LED reflective bracket needs to reflect the light emitted by the LED chip through a certain angle to reduce light loss, and then pass through epoxy resin or silica gel and other packaging materials to form a light source for LED lighting or display.
- LED reflective bracket material is a core material of LED lighting, which is directly related to the performance and life of LED light source.
- the LED reflector bracket needs to be exposed at a temperature of 150-200°C for 6-10 hours.
- the packaged lamp beads are made into a display screen, they need to go through SMT, requiring LED brackets or lamp beads
- SMT packaging and SMT, there will be no deformation, and it will not be damaged under load, and the requirements for the adhesion of the LED bracket material are relatively high.
- the LED display light source has gradually developed towards a small-pitch display with a dot pitch below P2.
- the manufacture of small-pitch display brackets is gradually developing in the direction of thin walls, multiple mold cavities, and small size, which puts forward more stringent requirements for the fluidity, ultra-multi-cavity formability, and mechanical strength of LED reflective bracket materials.
- the brightness and contrast of the display screen are very important indicators.
- the most widely used solution in the market is the LED bracket produced by pure white LED reflective material.
- the surface needs to be screen-printed with black ink. The process is cumbersome, affects efficiency, and costs are high.
- the contrast and gray scale of the display is very important indicators.
- the wavelengths that the eyes of ordinary people can perceive are between 780 and 400nm.
- the short-wave blue light with a wavelength of 400 to 450nm is the most harmful to the retina.
- the blue light with this wavelength will increase the amount of toxins in the macular area of the eye and seriously threaten people's eye health.
- the LED full-color display light source is packaged by three chips of red (R), green (G), and blue (B).
- R red
- G green
- B blue
- the brightness of the blue chip is the lowest, that is, the contrast is the highest, so the LED light source bracket
- the blue light reflectivity of the chip will directly affect the overall contrast of the LED display.
- the anti-blue light of LED screens has been popularized to the LED screens of various mobile phones and TVs, but the general measure is to coat the surface of the screen with anti-blue light film, but this measure has the defects of fragile film and high cost.
- the purpose of the present invention is to overcome the above-mentioned technical defects and provide a semi-aromatic polyamide molding composite material with high contrast and high gray scale, which can meet the requirements of packaging process and long-term reliability.
- Another object of the present invention is to provide the application of the above-mentioned semi-aromatic polyamide molding compound.
- a semi-aromatic polyamide molding compound, by weight, comprising the following components:
- the 10T unit content is 80-95mol%, and the X unit is 5-20mol%; wherein, the X unit is composed of a diacid unit and a diamine unit, and the diacid unit is selected from terephthalic acid unit, m-phthalic acid unit At least one of dicarboxylic acid units, 1,6-adipic acid, and 1,10-sebacic acid units, and the diamine units are selected from 1,6-hexanediamine units, 1,9-nonanediamine unit, 2-methyl-1,5-pentanediamine unit, 2-methyl-1,8-octanediamine unit, 1,10-decanediamine unit, 1,12-dodecanediamine unit at least one;
- the average diameter of wollastonite is 4-20 ⁇ m, and the average length is 10-250 ⁇ m;
- the half maximum width ⁇ T 1/2 of the crystallization peak measured at a cooling rate of 20°C/min after heating up to 345°C by differential scanning calorimetry of the semi-aromatic polyamide molding compound is 4-11°C;
- the whiteness of the semi-aromatic polyamide molding composite material is less than 26.5, and the reflectance of 460nm light source is less than 6%.
- the X unit is not 10T.
- the PA10T/X resin is selected from at least one of PA10T/10I, PA10T/6T, PA10T/66, PA10T/1010, PA10T/610, PA10T/612, and PA10T/12T.
- the half maximum width ⁇ T 1/2 of the crystallization peak measured at a cooling rate of 20°C/min after heating up to 345°C by differential scanning calorimetry of the semi-aromatic polyamide molding compound is 5- 8°C.
- the PA10T/X resin of the present invention may be a commercially available product, or may be synthesized according to the following method.
- the PA10T/X used in the examples and comparative examples of the present invention is a self-made sample, and the raw materials such as reaction monomers and end-capping agents are from commercially available products.
- Pre-polymerization Add polymerization monomers (diacid, diamine), end-capping agent benzoic acid and deionized water in a stainless steel autoclave equipped with mechanical stirring. Vacuumize and replace with N2 for three times, then start to heat up and stir, raise the temperature to 170-190°C at a rate of 4-6°C/min, keep the temperature for 1-2 hours, then slowly Stir and keep the temperature for 3-5h to allow the pre-polymerization reaction to fully proceed. After the constant temperature is over, slowly increase the temperature to 270-290°C, and start to drain water to normal pressure. When the pressure drops to normal pressure, the drain valve is closed, the reaction is completed, and the material is discharged at room temperature.
- Solid-phase thickening put the material prepared in the pre-polymerization process into a vacuum drum, the drum speed is set at 10-15r/min, and the vacuum degree is set at 25-35Pa. Raise the temperature at a rate of 15-25°C/min. When the temperature reaches 260-270°C, take a sample to test the viscosity, and judge the end point of the discharge according to the viscosity (or number average molecular weight) result.
- the number average molecular weight of the PA10T/X resin is 1500-28000.
- the test method of the number average molecular weight is a conventional method, specifically: the number average molecular weight (Mn) of the PA10T/X resin sample is determined by gel permeation chromatography (GPC).
- GPC gel permeation chromatography
- the chromatographic workstation cirrus software was used to process the data to obtain the number average molecular weight distribution Mn.
- the average diameter of the wollastonite in the semi-aromatic polyamide molding composite resin matrix is 6-13 ⁇ m, and the average length is 80-120 ⁇ m.
- Wollastonite is a powder with a certain length-to-diameter ratio, and its microstructure is fibrous, and its length and diameter hardly change during the melting and shearing process in the screw.
- PA10T and wollastonite average diameter of 17 ⁇ m and average length of 180 ⁇ m
- solvent is used to dissolve the resin to test the average diameter and average length of wollastonite. It was found that the diameter of the wollastonite does not change in the shear of the screw, and the average length changes by about 0.5%.
- the toner is selected from at least one or more color mixed toners selected from carbon black, black species, and amorphous carbon toners.
- the toner is selected from amorphous carbon toner.
- the 460nm light source reflectance of the semi-aromatic polyamide molding compound is ⁇ 4.5%; more preferably, the 460nm light source reflectance of the semi-aromatic polyamide molding compound is ⁇ 3.8%.
- antioxidant selected from hindered phenol antioxidants, hindered amine antioxidants, phosphite antioxidants, mercaptan antioxidants agent, thiodipropionate antioxidant at least one.
- the application of the semi-aromatic polyamide molding composite material of the present invention is used for preparing a reflective support for a light source of an LED display screen.
- the preparation method of the semi-aromatic polyamide molding composite material of the present invention adding each component into a mixer and mixing evenly, and then extruding and granulating through a twin-screw extruder to obtain a semi-aromatic polyamide molding composite material; wherein The temperature range of the screw is 280-330°C, and the rotation speed is 450r/min.
- the reflectivity of the 460nm light source is mainly related to the surface roughness of the material (the greater the roughness of the surface of the object within a certain range, the diffuse reflection of the light emitted by the light source on the surface of the object, and the less light energy received at the light receiving end) ,
- the whiteness of the material is related (the lower the whiteness, the lower the reflectivity).
- the influence of the light source reflective support on the LED display screen on the gray scale and contrast of the LED display mainly lies in the whiteness and reflectivity of the light source reflective support.
- the semi-aromatic polyamide molding compound of the present invention is controlled by the following three aspects: whiteness ⁇ 26.5, 460nm light source reflectance is reduced to ⁇ 6% (increasing gray scale and contrast), and has long-term packaging stability (adhesion), the advantage of low blue light of the packaged LED screen.
- wollastonite can make the surface roughness of semi-aromatic polyamide molding composite parts meet the requirements of reducing 460nm light reflection, not only reduces the 460nm light source reflectivity, but also improves the closeness with hardware Compatibility.
- the preferred distribution size of wollastonite in the resin matrix can further reduce the reflectivity of the 460nm light source (reduce the blue light of the LED display screen), and improve the adhesion with hardware.
- the amorphous carbon toner can further reduce the whiteness and improve the light absorption, thereby reducing the reflectance of the 460nm light source.
- the crystallization peak FWHM of the semi-aromatic polyamide molding composite material is mainly adjusted by adjusting the addition amount and specification of the toner and wollastonite, and can also be adjusted by adjusting the number average of the semi-aromatic polyamide resin. The molecular weight is obtained.
- excellent adhesion can be obtained by adjusting the crystallization peak width at half maximum, wollastonite specification, and surface roughness of the PA10T/X molding compound.
- the semi-aromatic polyamide molding composite material of the present invention does not require additional spraying of light-absorbing paint or frosting, thereby reducing the cost of LED display light source brackets.
- the monomers used in the following polyamide polymerizations are commercially available and pure.
- PA10T/1010-1 10T unit content 80mol%, number average molecular weight 7500, crystalline peak width at half maximum ⁇ T 1/2 of 15.1°C, self-made by referring to some methods in the content of the invention;
- PA10T/1010-2 10T unit content 85mol%, number average molecular weight 9000, crystalline peak width at half maximum ⁇ T 1/2 of 16°C, self-made by referring to some methods in the content of the invention;
- PA10T/1010-3 10T unit content 90mol%, number average molecular weight 8500, crystalline peak width at half maximum ⁇ T 1/2 of 12.8°C, self-made by referring to some methods in the content of the invention;
- PA10T/1010-4 10T unit content 95mol%, number average molecular weight 13000, crystallization peak half maximum width ⁇ T 1/2 is 8.4 °C, self-made by referring to some methods in the content of the invention;
- PA10T/1010-5 10T unit content 90mol%, number average molecular weight 4300, crystalline peak width at half maximum ⁇ T 1/2 of 14.2°C, self-made by referring to some methods in the content of the invention;
- PA10T/1010-6 10T unit content 90mol%, number average molecular weight 21000, crystallization peak half-maximum width ⁇ T 1/2 is 18.3°C, self-made by referring to some methods in the content of the invention;
- PA10T/1010-7 10T unit content 75mol%, number average molecular weight 8800, crystallization peak half-maximum width ⁇ T 1/2 is 18.0°C, self-made by referring to some methods in the content of the invention;
- PA10T/1010-8 10T unit content 97mol%, number average molecular weight 8000, crystalline peak width at half maximum ⁇ T 1/2 of 7.5°C, self-made by referring to some methods in the content of the invention;
- PA10T/10I-1 10T unit content 80mol%, number average molecular weight 10500, crystallization peak half-maximum width ⁇ T 1/2 is 17.1 °C, self-made by referring to some methods in the content of the invention;
- PA10T/10I-2 10T unit content 85mol%, number average molecular weight 9800, crystallization peak half-maximum width ⁇ T 1/2 is 12°C, self-made by referring to some methods in the content of the invention;
- PA10T/10I-3 10T unit content 90mol%, number average molecular weight 8500, crystalline peak width at half maximum ⁇ T 1/2 of 8.3°C, self-made by referring to some methods in the content of the invention;
- PA10T/10I-4 10T unit content 95mol%, number average molecular weight 8000, crystallization peak half-maximum width ⁇ T 1/2 is 7.1 °C, self-made by referring to some methods in the content of the invention;
- PA10T/10I-5 10T unit content 60mol%, number average molecular weight 8000, crystallization peak half-maximum width ⁇ T 1/2 is 15°C, self-made by referring to some methods in the content of the invention;
- PA10T/66 The 10T unit content is 90mol%, the number average molecular weight is 8000, and the crystallization peak half maximum width ⁇ T 1/2 is 13.4°C. It is self-made by referring to some methods in the content of the invention.
- PA10T/12T 10T unit content 80mol%, number average molecular weight 8000, crystalline peak width at half maximum ⁇ T 1/2 of 10.6°C, self-made by referring to some methods in the content of the invention;
- Wollastonite A the average diameter is 4 ⁇ m, and the average length is 60 ⁇ m;
- Wollastonite B the average diameter is 6 ⁇ m, and the average length is 120 ⁇ m;
- Wollastonite C the average diameter is 13 ⁇ m, and the average length is 80 ⁇ m;
- Wollastonite D The average diameter is 17 ⁇ m, and the average length is 180 ⁇ m.
- the wollastonite used in the present invention is purchased from the market and screened to obtain the desired average diameter and average length range.
- Talc powder AH-1250, Guangxi Longsheng Huamei Talc Development Co., Ltd.
- Toner A Amorphous carbon toner N774, Tianjin Tianyang Qiushi Chemical Technology Co., Ltd.;
- Toner B carbon black M570, Cabot Chemical Co., Ltd.;
- Toner C Black Seed UN2014, Cabot Chemical Co., Ltd.;
- Toner D Mazcol Blue 153K, Shenzhen Dingtai Chemical Co., Ltd.
- Antioxidant Irganox1098, hindered phenolic antioxidant.
- Adhesiveness PA10T/X molded composite material sample passed the red ink test to characterize the adhesiveness of the bracket plastic and hardware: the LED display light source bracket material and the electroplated hardware belt are injected into the LED reflective cup , soak into the red ink, make the red ink soak the pins, place it, and observe whether there is red ink seeping into the inside of the reflective cup.
- the seal level is judged as A level
- the density level is D, it proves that the adhesion between the plastic and the hardware is poor, and there is a risk of causing the lamp bead to fail. On the contrary, if the density level is A, B, C, the packaged lamp bead has excellent airtightness and good reliability.
- the contrast of the evaluation material is characterized by the whiteness index of the material: a test piece with a length of 60 mm, a width of 60 mm, and a thickness of 1 mm prepared by injection molding the PA10T molding composite material.
- W H 100-[(100-L) 2 +a 2 +b 2 ] 1/2 .
- Reflectance a test piece with a length of 60 mm, a width of 60 mm, and a thickness of 1 mm prepared by injection molding the PA10T/X molding composite material. Use a Color Eye 7000A color difference meter to measure the reflectance of the test piece to light with a wavelength of 460nm.
- Table 1 Components (parts by weight) and test results of semi-aromatic polyamide molding composites in Examples 1-6
- Example 1 Example 2
- Example 3 Example 4
- Example 5 Example 6 PA10T/1010-1 60 60 60 60 60 Wollastonite A 30 35 40 45 50 60 Toner A 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Crystallization peak width at half maximum ⁇ T 1/2 , °C 10.6 9.3 8.8 8.1 7.5 7.2
- Adhesion level B B B B A BaiDu 26.03 25.77 25.28 24.67 24.01 24.32 Reflectivity,% 5.89 5.44 4.91 4.30 3.81 3.92
- Example 7 Example 8
- Example 9 Example 10
- Example 11 PA10T/1010-1 60 60 60 60 40 75 Wollastonite A 45 45 45 45 30 60 Toner A 1 1.3 1.8 0.5 1 4.5 Toner D the the the 0.8 the the the Crystallization peak width at half maximum ⁇ T 1/2 , °C 8.0 8.0 8.1 7.9 7.7 antioxidant the the the the the the 0.5 Adhesion level B B B B A A BaiDu 22.80 22.26 21.47 23.08 22.37 20.16 Reflectivity,% 3.36 2.94 2.61 3.15 3.08 2.35
- Example 13 Example 14
- Example 15 Example 16
- PA10T/1010-1 60 60 60
- Wollastonite A the the the 45 45 Wollastonite B
- the Wollastonite C the 45 the the the Wollastonite D
- the 45 the the Toner A 0.5 0.5 0.5 the the Toner B
- Toner C the the the the 0.5 Crystallization peak width at half maximum ⁇ T 1/2 , °C 8.2 8.5 8.9 8.1 8.1 Adhesion level A
- Adhesion level A A B B B BaiDu 24.28 24.05 24.48 24.89 25.33 Reflectivity,% 3.93 3.69 4.42 4.60 5.13
- the average diameter of wollastonite is preferably 6-14 ⁇ m, and the average length is 80-120 ⁇ m. It can further improve the adhesion level and reduce the reflectivity; the toner is preferably amorphous carbon toner.
- Table 4 Components (parts by weight) and test results of semi-aromatic polyamide molding composites in Examples 18-24
- Example 23 Example 24
- Example 25 Example 26
- PA10T/10I-1 60 the the the PA10T/10I-2 the 60 the the PA10T/10I-3 the the 60 the PA10T/10I-4 the the the 60 Wollastonite A 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45 45
- Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4 Comparative example 5 Comparative example 6 PA10T/1010-7 60 the the the the the PA10T/1010-8 the 60 the the the the PA10T/10I-5 the the 60 the the the PA10T/1010-1 the the 60 60 60
- Comparative example 7 Comparative example 8 PA10T/1010-1 60 60 Wollastonite A 35 35 Toner A 0.2 5 Crystallization peak width at half maximum ⁇ T 1/2 , °C 9.3 9.0 Adhesion level B C BaiDu 28.11 21.75 Reflectivity,% 6.41 6.50
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Abstract
Description
实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 实施例6 | |
PA10T/1010-1 | 60 | 60 | 60 | 60 | 60 | 60 |
硅灰石A | 30 | 35 | 40 | 45 | 50 | 60 |
色粉A | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
结晶峰半高宽ΔT 1/2,℃ | 10.6 | 9.3 | 8.8 | 8.1 | 7.5 | 7.2 |
密合等级 | B | B | B | B | A | A |
白度 | 26.03 | 25.77 | 25.28 | 24.67 | 24.01 | 24.32 |
反射率,% | 5.89 | 5.44 | 4.91 | 4.30 | 3.81 | 3.92 |
实施例7 | 实施例8 | 实施例9 | 实施例10 | 实施例11 | 实施例12 | |
PA10T/1010-1 | 60 | 60 | 60 | 60 | 40 | 75 |
硅灰石A | 45 | 45 | 45 | 45 | 30 | 60 |
色粉A | 1 | 1.3 | 1.8 | 0.5 | 1 | 4.5 |
色粉D | 0.8 | |||||
结晶峰半高宽ΔT 1/2,℃ | 8.0 | 8.0 | 8.0 | 8.1 | 7.9 | 7.7 |
抗氧剂 | 0.5 | |||||
密合等级 | B | B | B | B | A | A |
白度 | 22.80 | 22.26 | 21.47 | 23.08 | 22.37 | 20.16 |
反射率,% | 3.36 | 2.94 | 2.61 | 3.15 | 3.08 | 2.35 |
实施例13 | 实施例14 | 实施例15 | 实施例16 | 实施例17 | |
PA10T/1010-1 | 60 | 60 | 60 | 60 | 60 |
硅灰石A | 45 | 45 | |||
硅灰石B | 45 | ||||
硅灰石C | 45 | ||||
硅灰石D | 45 | ||||
色粉A | 0.5 | 0.5 | 0.5 | ||
色粉B | 0.5 |
色粉C | 0.5 | ||||
结晶峰半高宽ΔT 1/2,℃ | 8.2 | 8.5 | 8.9 | 8.1 | 8.1 |
密合等级 | A | A | B | B | B |
白度 | 24.28 | 24.05 | 24.48 | 24.89 | 25.33 |
反射率,% | 3.93 | 3.69 | 4.42 | 4.60 | 5.13 |
实施例23 | 实施例24 | 实施例25 | 实施例26 | |
PA10T/10I-1 | 60 | |||
PA10T/10I-2 | 60 | |||
PA10T/10I-3 | 60 | |||
PA10T/10I-4 | 60 | |||
硅灰石A | 45 | 45 | 45 | 45 |
色粉A | 0.5 | 0.5 | 0.5 | 0.5 |
结晶峰半高宽ΔT 1/2,℃ | 8.9 | 6.6 | 4.3 | 4.1 |
密合等级 | B | A | B | B |
白度 | 24.84 | 24.15 | 24.79 | 24.89 |
反射率,% | 4.29 | 3.80 | 4.32 | 4.41 |
对比例1 | 对比例2 | 对比例3 | 对比例4 | 对比例5 | 对比例6 | |
PA10T/1010-7 | 60 | |||||
PA10T/1010-8 | 60 | |||||
PA10T/10I-5 | 60 | |||||
PA10T/1010-1 | 60 | 60 | 60 |
硅灰石A | 45 | 45 | 45 | 20 | 70 | |
滑石粉 | 45 | |||||
色粉A | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
结晶峰半高宽ΔT 1/2,℃ | 9.6 | 3.9 | 8.2 | 9.6 | 11.2 | 6.8 |
密合等级 | C | D | D | D | D | C |
白度 | 26.90 | 24.81 | 30.14 | 28.49 | 27.84 | 27.40 |
反射率,% | 6.22 | 4.82 | 8.60 | 10.39 | 6.86 | 6.75 |
对比例7 | 对比例8 | |
PA10T/1010-1 | 60 | 60 |
硅灰石A | 35 | 35 |
色粉A | 0.2 | 5 |
结晶峰半高宽ΔT 1/2,℃ | 9.3 | 9.0 |
密合等级 | B | C |
白度 | 28.11 | 21.75 |
反射率,% | 6.41 | 6.50 |
Claims (10)
- 一种半芳香聚酰胺模塑复合材料,其特征在于,按重量份计,包括以下组分:PA10T/X树脂 40-75份;硅灰石 30-60份;色粉 0.5-4.5份;基于PA10T/X摩尔百分比计,10T单元含量80-95mol%,X单元5-20mol%;其中,X单元由二酸单元和二胺单元构成,二酸单元选自对苯二甲酸单元、间苯二甲酸单元、1,6-己二酸、1,10-癸二酸单元中的至少一种,所述的二胺单元选自1,6-己二胺单元、1,9-壬二胺单元、2-甲基-1,5-戊二胺单元、2-甲基-1,8-辛二胺单元、1,10-癸二胺单元、1,12-十二碳二胺单元中至少一种;在半芳香聚酰胺模塑复合材料树脂基体中,硅灰石的平均直径为4-20μm,平均长度为10-250μm;所述的半芳香聚酰胺模塑复合材料通过差示扫描量热法,升温至345℃后以20℃/min的降温速率测得的结晶峰半高宽ΔT 1/2为4-11℃;所述的半芳香聚酰胺模塑复合材料的白度<26.5,460nm光源反射率<6%。
- 根据权利要求1所述的半芳香聚酰胺模塑复合材料,其特征在于,所述的PA10T/X树脂选自PA10T/10I、PA10T/6T、PA10T/66、PA10T/1010、PA10T/610、PA10T/612、PA10T/12T中的至少一种。
- 根据权利要求1所述的半芳香聚酰胺模塑复合材料,其特征在于,所述的半芳香聚酰胺模塑复合材料通过差示扫描量热法,升温至345℃后以20℃/min的降温速率测得的结晶峰半高宽ΔT 1/2为5-8℃。
- 根据权利要求1所述的半芳香聚酰胺模塑复合材料,其特征在于,所述的PA10T/X树脂的数均分子量为1500-28000。
- 根据权利要求1所述的半芳香聚酰胺模塑复合材料,其特征在于,所述的硅灰石在半芳香聚酰胺模塑复合材料树脂基体中的平均直径为6-13μm,平均长度为80-120μm。
- 根据权利要求1所述的半芳香聚酰胺模塑复合材料,其特征在于,所述的色粉选自炭黑、黑种、无定形碳色粉中的至少一种或多种颜色混合色粉;优选的,所述的色粉选自无定形碳色粉。
- 根据权利要求1所述的半芳香聚酰胺模塑复合材料,其特征在于,优选的,所述的半芳香聚酰胺模塑复合材料的460nm光源反射率<4.5%;更优选,所述的半芳香聚酰胺模塑复合材料的460nm光源反射率<3.8%。
- 根据权利要求1所述的半芳香聚酰胺模塑复合材料,其特征在于,按重量份计,还包括0-3份抗氧剂。
- 权利要求1-8任一项所述半芳香聚酰胺模塑复合材料的制备方法,其特征在于,包括以下步骤,将各组分加入混料机中混合均匀,再通过双螺杆挤出机挤出造粒,得到半芳香聚酰胺模塑复合材料;其中螺杆温度范围280-330℃、转速为400-500r/min。
- 权利要求1-8任一项所述的半芳香聚酰胺模塑复合材料的应用,其特征在于,用于制备LED显示屏光源反射支架。
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US20190002638A1 (en) * | 2017-01-20 | 2019-01-03 | Kingfa Sci. & Tech. Co., Ltd. | Semiaromatic polyamide resin and preparation method thereof and polyamide molding composition consisting of the same |
CN108383996A (zh) * | 2018-01-10 | 2018-08-10 | 金发科技股份有限公司 | 一种高结晶速率聚酰胺及其制备方法和应用 |
CN110294842A (zh) * | 2019-05-24 | 2019-10-01 | 金发科技股份有限公司 | 一种半芳香族聚酰胺及其合成方法和由其组成的聚酰胺模塑组合物 |
WO2021204600A1 (en) * | 2020-04-09 | 2021-10-14 | Basf Se | Polyamide composition for optical elements |
CN112358610A (zh) * | 2020-05-28 | 2021-02-12 | 金发科技股份有限公司 | 一种聚酰胺和由其组成的聚酰胺模塑组合物 |
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