CN113004688A - Preparation process of high-performance polyamide composite material for halogen-free flame-retardant LED - Google Patents
Preparation process of high-performance polyamide composite material for halogen-free flame-retardant LED Download PDFInfo
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- CN113004688A CN113004688A CN202110156699.0A CN202110156699A CN113004688A CN 113004688 A CN113004688 A CN 113004688A CN 202110156699 A CN202110156699 A CN 202110156699A CN 113004688 A CN113004688 A CN 113004688A
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 50
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 229920006130 high-performance polyamide Polymers 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000004611 light stabiliser Substances 0.000 claims abstract description 13
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 11
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 claims abstract description 11
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 9
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 9
- 239000002667 nucleating agent Substances 0.000 claims abstract description 9
- 239000006057 Non-nutritive feed additive Substances 0.000 claims abstract description 8
- 229920006012 semi-aromatic polyamide Polymers 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 4
- 229920006154 PA11T Polymers 0.000 claims description 3
- XSAOTYCWGCRGCP-UHFFFAOYSA-K aluminum;diethylphosphinate Chemical compound [Al+3].CCP([O-])(=O)CC.CCP([O-])(=O)CC.CCP([O-])(=O)CC XSAOTYCWGCRGCP-UHFFFAOYSA-K 0.000 claims 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 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- BNEMLSQAJOPTGK-UHFFFAOYSA-N zinc;dioxido(oxo)tin Chemical compound [Zn+2].[O-][Sn]([O-])=O BNEMLSQAJOPTGK-UHFFFAOYSA-N 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- 229920000388 Polyphosphate Polymers 0.000 claims description 2
- 125000001931 aliphatic group Chemical group 0.000 claims description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 239000003963 antioxidant agent Substances 0.000 claims description 2
- 150000001805 chlorine compounds Chemical group 0.000 claims description 2
- 238000000354 decomposition reaction Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- 239000000314 lubricant Substances 0.000 claims description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- GKTNLYAAZKKMTQ-UHFFFAOYSA-N n-[bis(dimethylamino)phosphinimyl]-n-methylmethanamine Chemical compound CN(C)P(=N)(N(C)C)N(C)C GKTNLYAAZKKMTQ-UHFFFAOYSA-N 0.000 claims description 2
- 229920006119 nylon 10T Polymers 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229920006115 poly(dodecamethylene terephthalamide) Polymers 0.000 claims description 2
- 229920006139 poly(hexamethylene adipamide-co-hexamethylene terephthalamide) Polymers 0.000 claims description 2
- 229920006131 poly(hexamethylene isophthalamide-co-terephthalamide) Polymers 0.000 claims description 2
- 229920006128 poly(nonamethylene terephthalamide) Polymers 0.000 claims description 2
- 239000001205 polyphosphate Substances 0.000 claims description 2
- 235000011176 polyphosphates Nutrition 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- XAEWLETZEZXLHR-UHFFFAOYSA-N zinc;dioxido(dioxo)molybdenum Chemical compound [Zn+2].[O-][Mo]([O-])(=O)=O XAEWLETZEZXLHR-UHFFFAOYSA-N 0.000 claims description 2
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims 1
- 239000012964 benzotriazole Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 12
- 230000007547 defect Effects 0.000 abstract description 2
- 238000004383 yellowing Methods 0.000 abstract description 2
- 235000010215 titanium dioxide Nutrition 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 229920006375 polyphtalamide Polymers 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- KGRVJHAUYBGFFP-UHFFFAOYSA-N 2,2'-Methylenebis(4-methyl-6-tert-butylphenol) Chemical compound CC(C)(C)C1=CC(C)=CC(CC=2C(=C(C=C(C)C=2)C(C)(C)C)O)=C1O KGRVJHAUYBGFFP-UHFFFAOYSA-N 0.000 description 1
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 description 1
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 150000001565 benzotriazoles Chemical class 0.000 description 1
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 1
- 239000008116 calcium stearate Substances 0.000 description 1
- 235000013539 calcium stearate Nutrition 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
Classifications
-
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic 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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3472—Five-membered rings
- C08K5/3475—Five-membered rings condensed with carbocyclic rings
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5313—Phosphinic compounds, e.g. R2=P(:O)OR'
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/5399—Phosphorus bound to nitrogen
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/08—Oxygen-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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2244—Oxides; Hydroxides of metals of zirconium
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The application discloses a preparation process of a high-performance polyamide composite material for a halogen-free flame-retardant LED, which sequentially comprises the following steps: s1, preparing the following raw materials in parts by weight: 30-50 parts of semi-aromatic polyamide, 5-20 parts of halogen-free flame retardant, 1-5 parts of flame retardant synergist, 5-25 parts of titanium dioxide, 5-25 parts of potassium titanate whisker, 1-15 parts of nano metal oxide, 0.1-5 parts of light stabilizer, 0.1-2 parts of nucleating agent and 0.1-5 parts of processing aid; s2, mixing the semi-aromatic polyamide, the nucleating agent, the light stabilizer and the processing aid by a high-speed mixer, then adding the mixture from a main feed opening of a double-screw extruder, mixing the titanium dioxide, the nano metal oxide and the potassium titanate whisker by the high-speed mixer, then adding the mixture from a side feed opening of the double-screw extruder, mixing the halogen-free flame retardant and the flame-retardant synergist by the high-speed mixer, and then adding the mixture from a feed opening at the other side of the double-screw extruder; s3, melt mixing, extruding and granulating. The invention further improves the light resistance of the material, so that the material is not easy to have the defects of yellowing and the like.
Description
Technical Field
The invention relates to the field of composite materials, in particular to a preparation process of a high-performance polyamide composite material for a halogen-free flame-retardant LED.
Background
The LED reflecting support material has great influence on the brightness and the service life of an LED light source and is a core material in the LED illumination and display industry. Therefore, the material for the LED reflection bracket needs to have: the crystallization rate is high, and the molding processing is easy; the strength is high; the dimensional stability is good; good temperature and moisture resistance and the like.
PPA has the advantages of short molding cycle, high strength, good heat resistance and dimensional stability and relatively low cost, so that the PPA still occupies a mainstream position in the market relative to PCT and EMC materials.
With the continuous development of the LED industry, the requirements on the brightness and the heat resistance of the LED reflecting bracket material are higher and higher; the rapid development of small-spacing LED products strengthens the performance requirements on the crystallinity and the dimensional stability of LED reflecting support materials. In addition, for safety, the material needs to have good flame retardancy, and the conventional halogen-containing flame retardant generates toxic substances when burning, thereby seriously harming human health and causing environmental pollution. Therefore, the halogen-free flame-retardant high-performance polyamide composite material is the most potential LED reflection bracket material at present.
Disclosure of Invention
The invention aims to provide a preparation process of a high-performance polyamide composite material for a halogen-free flame-retardant LED, which adopts polyamide as matrix resin, and adds a long-acting light stabilizer to further improve the light resistance of the material, so that the material is not easy to have the defects of yellowing and the like; the crystallization performance of the material is improved by utilizing the shading and whitening effects of titanium dioxide and nano metal oxide and adding a heterogeneous nucleating agent; the halogen-free flame retardant and the flame retardant synergist are added to achieve the halogen-free flame retardant effect.
In order to achieve the above object, the present invention provides the following technical solutions.
The embodiment of the application discloses a preparation process of a high-performance polyamide composite material for a halogen-free flame-retardant LED, which sequentially comprises the following steps:
s1, preparing the following raw materials in parts by weight: 30-50 parts of semi-aromatic polyamide, 5-20 parts of halogen-free flame retardant,
1-5 parts of flame-retardant synergist, 5-25 parts of titanium dioxide, 5-25 parts of potassium titanate whisker, 1-15 parts of nano metal oxide, 0.1-5 parts of light stabilizer, 0.1-2 parts of nucleating agent and 0.1-5 parts of processing aid;
s2, mixing the semi-aromatic polyamide, the nucleating agent, the light stabilizer and the processing aid by a high-speed mixer, then adding the mixture from a main feed opening of a double-screw extruder, mixing the titanium dioxide, the nano metal oxide and the potassium titanate whisker by the high-speed mixer, then adding the mixture from a side feed opening of the double-screw extruder, mixing the halogen-free flame retardant and the flame-retardant synergist by the high-speed mixer, and then adding the mixture from a feed opening at the other side of the double-screw extruder;
s3, carrying out melt mixing extrusion granulation, wherein the return rotation speed of each high-speed mixer is 60-120 rpm, the mixing time is 5-10 min, the output of the double-screw extruder is 50-200 Kg/h, the rotation speed is 100-300 rpm, the temperature of each section of the machine barrel is 300 +/-20 ℃, the head temperature is 310 +/-10 ℃, and the extraction pressure of the vacuum section is-0.08 +/-0.02 MPa.
Preferably, in the preparation process of the high-performance polyamide composite material for the halogen-free flame-retardant LED, the semi-aromatic polyamide is one or more of PA6T/66, PA6T/6I, PA9T, PA10T, PA11T and PA 12T.
Preferably, in the preparation process of the high-performance polyamide composite material for the halogen-free flame-retardant LED, the halogen-free flame retardant is at least one of aluminum diethylphosphinate, phosphazene flame retardant and melamine polyphosphate.
Preferably, in the preparation process of the high-performance polyamide composite material for the halogen-free flame-retardant LED, the flame-retardant synergist is at least one of zinc stannate, zinc molybdate, antimony trioxide and aluminum hydroxide.
It is preferable thatIn the preparation process of the high-performance polyamide composite material for the halogen-free flame-retardant LED, the titanium dioxide is chloride rutile titanium dioxide, D is 500.1-0.5 mu m, and the BET specific surface area is 10-20 m2/g。
Preferably, in the preparation process of the high-performance polyamide composite material for the halogen-free flame-retardant LED, the length of the potassium titanate whisker fiber is 5-30 μm, and the fiber diameter is 0.1-2 μm.
Preferably, in the preparation process of the high-performance polyamide composite material for the halogen-free flame-retardant LED, the nano metal oxide is one or more of zinc oxide, aluminum oxide and zirconium oxide.
Preferably, in the preparation process of the high-performance polyamide composite material for the halogen-free flame-retardant LED, the light stabilizer is one or more of benzotriazoles and hindered amine light stabilizers, and the 5% decomposition temperature of the light stabilizer is more than 300 ℃.
Preferably, in the preparation process of the high-performance polyamide composite material for the halogen-free flame-retardant LED, the nucleating agent is superfine talcum powder, the particle size is 1-5 μm, and the pH value is 8-10.
Preferably, in the preparation process of the high-performance polyamide composite material for the halogen-free flame-retardant LED, the processing aid comprises antioxidants 168 and 1098 and an aliphatic metal salt lubricant.
Detailed Description
Technical solutions in the embodiments of the present invention will be described in detail below, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The formulations of example 1 and example 2 are as follows (in parts by mass):
| components | Example 1 | Example 2 |
| PA11T | 45.5 | 48.5 |
| Aluminium diethylphosphinate | 15 | - |
| Phosphazene flame retardants | - | 12 |
| Zinc stannate | 1 | 1 |
| Titanium white powder | 10 | 10 |
| Potassium titanate whisker | 20 | 20 |
| Nano zirconium oxide | 5 | 5 |
| Talcum powder | 1 | 1 |
| Sodium benzoate | 1 | 1 |
| Polymeric carbonized diamines | 0.3 | 0.3 |
| Methylene bis [ 6-benzotriazole-4-tert-octylphenol] | 0.2 | 0.2 |
| Antioxidant 1098 | 0.2 | 0.2 |
| Antioxidant 168 | 0.3 | 0.3 |
| Calcium stearate | 0.5 | 0.5 |
The performance of the composite material prepared by the invention reaches the following level, and the whiteness, the flame retardance and the crystallinity are superior to those of a comparative example (PPA/15 percent titanium dioxide/20 percent potassium titanate whisker)
| Item | Example 1 | Example 2 | Comparative example |
| Tensile strength MPa | 120 | 125 | 130 |
| Bending strength MPa | 175 | 180 | 190 |
| Whiteness degree | 95 | 95 | 92 |
| Molding shrinkage percentage% | 0.15 | 0.15 | 0.15 |
| UL94 flame retardant Properties | V-0 | V-0 | HB |
| Crystallization temperature C | 280 | 280 | 270 |
The present embodiments are to be considered as illustrative and not restrictive, and the scope of the patent is to be determined by the appended claims.
Claims (10)
1. A preparation process of a high-performance polyamide composite material for a halogen-free flame-retardant LED is characterized by sequentially comprising the following steps of:
s1, preparing the following raw materials in parts by weight: 30-50 parts of semi-aromatic polyamide, 5-20 parts of halogen-free flame retardant,
1-5 parts of flame-retardant synergist, 5-25 parts of titanium dioxide, 5-25 parts of potassium titanate whisker, 1-15 parts of nano metal oxide, 0.1-5 parts of light stabilizer, 0.1-2 parts of nucleating agent and 0.1-5 parts of processing aid;
s2, mixing the semi-aromatic polyamide, the nucleating agent, the light stabilizer and the processing aid by a high-speed mixer, then adding the mixture from a main feed opening of a double-screw extruder, mixing the titanium dioxide, the nano metal oxide and the potassium titanate whisker by the high-speed mixer, then adding the mixture from a side feed opening of the double-screw extruder, mixing the halogen-free flame retardant and the flame-retardant synergist by the high-speed mixer, and then adding the mixture from a feed opening at the other side of the double-screw extruder;
s3, carrying out melt mixing extrusion granulation, wherein the return rotation speed of each high-speed mixer is 60-120 rpm, the mixing time is 5-10 min, the output of the double-screw extruder is 50-200 Kg/h, the rotation speed is 100-300 rpm, the temperature of each section of the machine barrel is 300 +/-20 ℃, the head temperature is 310 +/-10 ℃, and the extraction pressure of the vacuum section is-0.08 +/-0.02 MPa.
2. The preparation process of the high-performance polyamide composite material for the halogen-free flame-retardant LED according to claim 1, wherein the semi-aromatic polyamide is one or more of PA6T/66, PA6T/6I, PA9T, PA10T, PA11T and PA 12T.
3. The preparation process of the halogen-free flame retardant high-performance polyamide composite material for the LED according to claim 1, wherein the halogen-free flame retardant is at least one of aluminum diethylphosphinate, phosphazene flame retardant and melamine polyphosphate.
4. The preparation process of the halogen-free flame-retardant high-performance polyamide composite material for the LED according to claim 1, wherein the flame-retardant synergist is at least one of zinc stannate, zinc molybdate, antimony trioxide and aluminum hydroxide.
5. The preparation process of the halogen-free flame-retardant high-performance polyamide composite material for the LED according to claim 1, wherein the titanium dioxide is chloride rutile type titanium dioxide, D is 500.1-0.5 μm, and BET specific surface area is 10-20 m2/g。
6. The preparation process of the halogen-free flame-retardant high-performance polyamide composite material for the LED according to claim 1, wherein the length of the potassium titanate whisker fiber is 5-30 μm, and the fiber diameter is 0.1-2 μm.
7. The preparation process of the halogen-free flame-retardant high-performance polyamide composite material for the LED according to claim 1, wherein the nano metal oxide is one or more of zinc oxide, aluminum oxide and zirconium oxide.
8. The preparation process of the halogen-free flame-retardant high-performance polyamide composite material for the LED according to claim 1, wherein the light stabilizer is one or more of benzotriazole and hindered amine light stabilizers, and the 5% decomposition temperature of the light stabilizer is more than 300 ℃.
9. The preparation process of the halogen-free flame-retardant high-performance polyamide composite material for the LED according to claim 1, wherein the nucleating agent is superfine talcum powder, the particle size is 1-5 μm, and the pH value is 8-10.
10. The preparation process of the halogen-free flame-retardant high-performance polyamide composite material for the LED according to claim 1, wherein the processing aid comprises antioxidants 168 and 1098 and an aliphatic metal salt lubricant.
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