CN114957985A - Preparation method of microcapsule phosphazene flame retardant-based halogen-free flame-retardant polyamide composite material - Google Patents
Preparation method of microcapsule phosphazene flame retardant-based halogen-free flame-retardant polyamide composite material Download PDFInfo
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- CN114957985A CN114957985A CN202210688303.1A CN202210688303A CN114957985A CN 114957985 A CN114957985 A CN 114957985A CN 202210688303 A CN202210688303 A CN 202210688303A CN 114957985 A CN114957985 A CN 114957985A
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- flame retardant
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 89
- 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 75
- 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 title claims abstract description 41
- 239000004952 Polyamide Substances 0.000 title claims abstract description 33
- 229920002647 polyamide Polymers 0.000 title claims abstract description 33
- 239000003094 microcapsule Substances 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 239000004611 light stabiliser Substances 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 10
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000006057 Non-nutritive feed additive Substances 0.000 claims abstract description 8
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 8
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 8
- 239000002667 nucleating agent 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 4
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 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
- 239000003822 epoxy resin Substances 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 3
- 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 claims description 2
- 229920006154 PA11T Polymers 0.000 claims description 2
- 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 claims description 2
- 125000001931 aliphatic group Chemical group 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 150000001565 benzotriazoles Chemical class 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 238000000354 decomposition reaction Methods 0.000 claims description 2
- 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 2
- 238000001035 drying 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
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 238000000034 method Methods 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
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 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
- 239000000376 reactant Substances 0.000 claims description 2
- 238000010992 reflux Methods 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 238000005406 washing Methods 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
- BNEMLSQAJOPTGK-UHFFFAOYSA-N zinc;dioxido(oxo)tin Chemical compound [Zn+2].[O-][Sn]([O-])=O BNEMLSQAJOPTGK-UHFFFAOYSA-N 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- VEORPZCZECFIRK-UHFFFAOYSA-N 3,3',5,5'-tetrabromobisphenol A Chemical compound C=1C(Br)=C(O)C(Br)=CC=1C(C)(C)C1=CC(Br)=C(O)C(Br)=C1 VEORPZCZECFIRK-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- WHHGLZMJPXIBIX-UHFFFAOYSA-N decabromodiphenyl ether Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1OC1=C(Br)C(Br)=C(Br)C(Br)=C1Br WHHGLZMJPXIBIX-UHFFFAOYSA-N 0.000 description 2
- 239000012796 inorganic flame retardant Substances 0.000 description 2
- QKORWYWGMJCFAW-UHFFFAOYSA-N 2-phenyl-3h-1,3,2-benzoxazaphosphinin-4-one Chemical compound O1C2=CC=CC=C2C(=O)NP1C1=CC=CC=C1 QKORWYWGMJCFAW-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229920006375 polyphtalamide Polymers 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The application discloses a preparation method of a halogen-free flame-retardant polyamide composite material based on a microcapsule phosphazene flame retardant, which sequentially comprises the following steps: s1, preparing the following raw materials in parts by weight: 50-70 parts of semi-aromatic polyamide, 10-20 parts of microcapsule phosphazene flame retardant, 1-5 parts of flame retardant synergist, 20-40 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 other processing aids; s2, mixing the semi-aromatic polyamide, the light stabilizer, the nucleating agent and other processing aids through a high-speed mixer, then adding the mixture from a main feed opening of a double-screw extruder, mixing the nano metal oxide and the potassium titanate whisker through the high-speed mixer, then adding the mixture from a first side feed opening of the double-screw extruder, mixing the microcapsule phosphazene flame retardant and the flame retardant synergist through the high-speed mixer, and then adding the mixture from a second side feed opening of the double-screw extruder; s3, melt mixing, extruding and granulating. The invention can meet the requirements on the performance of polyamide in the electronic and electric industry.
Description
Technical Field
The invention relates to the field of composite materials, and particularly relates to a preparation method of a halogen-free flame-retardant polyamide composite material based on a microcapsule phosphazene flame retardant.
Background
The high-temperature resistant polyamide material in the current market still occupies the mainstream position in the electronic and electric industry due to the advantages of short forming period, high strength, good heat resistance and dimensional stability and relatively low cost. For safety reasons, the material needs to have good flame retardancy in order to prevent short-circuiting of the circuit or the occurrence of fire due to local temperature rise. Flame retardants commonly used in polyamides include halogen-based flame retardants such as tetrabromobisphenol A (TBBPA), decabromodiphenyl oxide (DBOPO), and polydibromophenyl ether (PDBPO), among others. The halogen flame retardant can effectively improve the flame retardance of the alloy, but generates a large amount of corrosive gas during combustion to cause secondary damage. Inorganic flame retardants, such as aluminum hydroxide and magnesium hydroxide, have low flame retardant efficiency and high addition levels, and have adverse effects on the mechanical properties of the alloy.
The traditional halogen-containing flame retardant can generate toxic substances during combustion, seriously harms human health and causes environmental pollution. The inorganic flame retardant has low flame retardant efficiency and high addition amount, and has adverse effect on the alloy performance. And the flame retardant is directly melt-blended with polyamide to hardly obtain a good dispersion effect, so that the flame retardance is unstable and potential safety hazards still exist. Microencapsulation of the flame retardant is an efficient method for easily and uniformly dispersing the flame retardant in the resin.
CN111607221A adopts in-situ coated red phosphorus flame retardant to prepare flame-retardant polyamide material. Red phosphorus is easy to react at high temperature to produce virulent phosphine gas, and has certain harm. In addition, the red phosphorus is dark red in appearance, has colorability on the prepared material, and limits the application range of the material.
Disclosure of Invention
The invention aims to provide a preparation method of a halogen-free flame-retardant polyamide composite material based on a microcapsule phosphazene flame retardant.
In order to achieve the above object, the present invention provides the following technical solutions.
The embodiment of the application discloses a preparation method of a halogen-free flame-retardant polyamide composite material based on a microcapsule phosphazene flame retardant, which sequentially comprises the following steps:
s1, preparing the following raw materials in parts by weight: 50-70 parts of semi-aromatic polyamide, 10-20 parts of microcapsule phosphazene flame retardant, 1-5 parts of flame retardant synergist, 20-40 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 other processing aids;
s2, mixing the semi-aromatic polyamide, the light stabilizer, the nucleating agent and other processing aids through a high-speed mixer, then adding the mixture from a main feed opening of a double-screw extruder, mixing the nano metal oxide and the potassium titanate whisker through the high-speed mixer, then adding the mixture from a first side feed opening of the double-screw extruder, mixing the microcapsule phosphazene flame retardant and the flame retardant synergist through the high-speed mixer, and then adding the mixture from a second side feed opening of the double-screw extruder;
s3, carrying out melt mixing extrusion granulation, wherein the rotating speed of a high-speed mixer is 60-120 rpm, the mixing time is 5-10 min, the output of a double-screw extruder is 50-200 Kg/h, the rotating speed is 100-300 rpm, the temperature of each section of a machine barrel is 300 +/-20 ℃, the head temperature is 310 +/-10 ℃, and the extraction pressure of a vacuum section is-0.08 +/-0.02 MPa.
Preferably, in the preparation method of the halogen-free flame retardant polyamide composite material based on the microcapsule phosphazene flame retardant, the semi-aromatic polyamide is one or more of PA6T/66, PA6T/6I, PA9T, PA10T, PA11T and PA 12T.
Preferably, in the preparation method of the halogen-free flame-retardant polyamide composite material based on the microcapsule phosphazene flame retardant, the microcapsule phosphazene flame retardant is prepared by microencapsulating the phosphazene flame retardant, and the particle size is 1-20 microns.
Preferably, in the preparation method of the halogen-free flame-retardant polyamide composite material based on the microencapsulated phosphazene flame retardant, the microencapsulation treatment sequentially comprises the following steps: dissolving a phosphazene flame retardant into a certain amount of acetone solvent in a reaction kettle, dissolving epoxy resin by using ethanol and acetone at room temperature, mixing and stirring the two solutions, gradually increasing the temperature to 50 ℃ after the two solutions are completely mixed, gradually dropwise adding a curing agent of the epoxy resin, continuously stirring in the reaction kettle, carrying out condensation reflux, keeping the reaction for about 5 hours, carrying out suction filtration on a reactant, washing, and drying to obtain the microencapsulated phosphazene flame retardant.
Preferably, in the preparation method of the microcapsule phosphazene flame retardant-based halogen-free flame retardant polyamide composite material, the flame retardant synergist comprises at least one of zinc stannate, zinc molybdate, antimony trioxide or aluminum hydroxide.
Preferably, in the preparation method of the halogen-free flame-retardant polyamide composite material based on the microcapsule phosphazene flame retardant, the potassium titanate whisker is a TISMO series produced by Japanese Otsuka chemistry, the fiber length is 5-30 μm, and the fiber diameter is 0.1-2 μm.
Preferably, in the preparation method of the halogen-free flame-retardant polyamide composite material based on the microencapsulated phosphazene flame retardant, the nano metal oxide comprises one or more of zinc oxide, aluminum oxide and zirconium oxide.
Preferably, in the preparation method of the halogen-free flame-retardant polyamide composite material based on the microcapsule phosphazene flame retardant, the light stabilizer comprises one or more of benzotriazoles and hindered amine light stabilizers, and the 5% decomposition temperature is more than 300 ℃.
Preferably, in the preparation method of the halogen-free flame-retardant polyamide composite material based on the microcapsule phosphazene flame retardant, 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 method of the microcapsule phosphazene flame retardant-based halogen-free flame retardant polyamide composite material, the other processing aids comprise an antioxidant 168, an antioxidant 1098 and an aliphatic metal salt lubricant.
Compared with the prior art, the phosphazene flame retardant is adopted as a raw material, and is microencapsulated through microcapsule treatment, and the flame retardant is suitable for high-temperature processing after microcapsule treatment and has the characteristics of no migration, low volatilization, high flame retardant efficiency and small influence on the mechanical property and heat resistance of a material; the halogen-free flame-retardant polyamide composite material is prepared by blending polyamide and the microcapsule phosphazene flame retardant by adopting a double-screw extruder, has excellent flame retardant property and mechanical property and good molding processability, and can meet the requirement on the performance of the polyamide in the electronic and electric industry.
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):
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/20 percent potassium titanate whisker/15 percent phosphazene flame retardant)
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 method of a halogen-free flame-retardant polyamide composite material based on a microcapsule phosphazene flame retardant is characterized by sequentially comprising the following steps:
s1, preparing the following raw materials in parts by weight: 50-70 parts of semi-aromatic polyamide, 10-20 parts of microcapsule phosphazene flame retardant, 1-5 parts of flame retardant synergist, 20-40 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 other processing aids;
s2, mixing the semi-aromatic polyamide, the light stabilizer, the nucleating agent and other processing aids through a high-speed mixer, then adding the mixture from a main feed opening of a double-screw extruder, mixing the nano metal oxide and the potassium titanate whisker through the high-speed mixer, then adding the mixture from a first side feed opening of the double-screw extruder, mixing the microcapsule phosphazene flame retardant and the flame retardant synergist through the high-speed mixer, and then adding the mixture from a second side feed opening of the double-screw extruder;
s3, carrying out melt mixing extrusion granulation, wherein the rotating speed of a high-speed mixer is 60-120 rpm, the mixing time is 5-10 min, the output of a double-screw extruder is 50-200 Kg/h, the rotating speed is 100-300 rpm, the temperature of each section of a machine barrel is 300 +/-20 ℃, the head temperature is 310 +/-10 ℃, and the extraction pressure of a vacuum section is-0.08 +/-0.02 MPa.
2. The preparation method of the microcapsule phosphazene flame retardant-based halogen-free flame retardant polyamide composite material 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 method of the microcapsule phosphazene flame retardant-based halogen-free flame retardant polyamide composite material according to claim 1, wherein the microcapsule phosphazene flame retardant is microencapsulated, and the particle size is 1-20 microns.
4. The preparation method of the microencapsulated phosphazene flame retardant-based halogen-free flame retardant polyamide composite material according to claim 3, wherein the microencapsulation treatment comprises the following steps in sequence: dissolving a phosphazene flame retardant into a certain amount of acetone solvent in a reaction kettle, dissolving epoxy resin by using ethanol and acetone at room temperature, mixing and stirring the two solutions, gradually increasing the temperature to 50 ℃ after the two solutions are completely mixed, gradually dropwise adding a curing agent of the epoxy resin, continuously stirring in the reaction kettle, carrying out condensation reflux, keeping the reaction for about 5 hours, carrying out suction filtration on a reactant, washing, and drying to obtain the microencapsulated phosphazene flame retardant.
5. The method for preparing the microencapsulated phosphazene flame retardant-based halogen-free flame retardant polyamide composite material according to claim 1, wherein the flame retardant synergist comprises at least one of zinc stannate, zinc molybdate, antimony trioxide or aluminum hydroxide.
6. The preparation method of the microcapsule phosphazene flame retardant-based halogen-free flame retardant polyamide composite material according to claim 1, wherein the potassium titanate whisker is of a TISMO series produced by japanese red jar chemistry, the fiber length is 5 to 30 μm, and the fiber diameter is 0.1 to 2 μm.
7. The preparation method of the microencapsulated phosphazene flame retardant-based halogen-free flame retardant polyamide composite material according to claim 1, wherein the nano metal oxide comprises one or more of zinc oxide, aluminum oxide and zirconium oxide.
8. The preparation method of the microencapsulated phosphazene flame retardant-based halogen-free flame retardant polyamide composite material according to claim 1, wherein the light stabilizer comprises one or more of benzotriazoles and hindered amine light stabilizers, and the 5% decomposition temperature is more than 300 ℃.
9. The preparation method of the microcapsule phosphazene flame retardant-based halogen-free flame retardant polyamide composite material 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 method of the microcapsule phosphazene flame retardant-based halogen-free flame retardant polyamide composite material according to claim 1, wherein the other processing aids comprise an antioxidant 168, an antioxidant 1098 and an aliphatic metal salt lubricant.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210688303.1A CN114957985A (en) | 2022-06-17 | 2022-06-17 | Preparation method of microcapsule phosphazene flame retardant-based halogen-free flame-retardant polyamide composite material |
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| CN202210688303.1A CN114957985A (en) | 2022-06-17 | 2022-06-17 | Preparation method of microcapsule phosphazene flame retardant-based halogen-free flame-retardant polyamide composite material |
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| CN110922749A (en) * | 2019-10-26 | 2020-03-27 | 张家港大塚化学有限公司 | Preparation method of high-weather-resistance and high-reflectivity polyamide composite material for LED |
| CN112646341A (en) * | 2020-11-27 | 2021-04-13 | 张家港大塚化学有限公司 | Preparation process of halogen-free flame-retardant, antistatic, high-wear-resistance and high-strength PC/ASA alloy |
| CN113004688A (en) * | 2021-02-04 | 2021-06-22 | 张家港大塚化学有限公司 | Preparation process of high-performance polyamide composite material for halogen-free flame-retardant LED |
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- 2022-06-17 CN CN202210688303.1A patent/CN114957985A/en active Pending
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| JP2017082229A (en) * | 2016-12-21 | 2017-05-18 | 株式会社伏見製薬所 | Microncapsulated flame retardant and flame retardant resin composition containing the same |
| CN110922749A (en) * | 2019-10-26 | 2020-03-27 | 张家港大塚化学有限公司 | Preparation method of high-weather-resistance and high-reflectivity polyamide composite material for LED |
| CN110883975A (en) * | 2019-11-06 | 2020-03-17 | 张家港大塚化学有限公司 | Preparation method of low-roughness high-CTI-value flame-retardant polyamide composite material |
| CN112646341A (en) * | 2020-11-27 | 2021-04-13 | 张家港大塚化学有限公司 | Preparation process of halogen-free flame-retardant, antistatic, high-wear-resistance and high-strength PC/ASA alloy |
| CN113004688A (en) * | 2021-02-04 | 2021-06-22 | 张家港大塚化学有限公司 | Preparation process of high-performance polyamide composite material for halogen-free flame-retardant LED |
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Application publication date: 20220830 |