CN115572480A - Polyamide composition and preparation method and application thereof - Google Patents
Polyamide composition and preparation method and application thereof Download PDFInfo
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- CN115572480A CN115572480A CN202211017806.2A CN202211017806A CN115572480A CN 115572480 A CN115572480 A CN 115572480A CN 202211017806 A CN202211017806 A CN 202211017806A CN 115572480 A CN115572480 A CN 115572480A
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- polyamide composition
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- polyamide
- aromatic polyamide
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- 239000000203 mixture Substances 0.000 title claims abstract description 73
- 229920002647 polyamide Polymers 0.000 title claims abstract description 72
- 239000004952 Polyamide Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229920006012 semi-aromatic polyamide Polymers 0.000 claims abstract description 49
- 238000002425 crystallisation Methods 0.000 claims abstract description 30
- 230000008025 crystallization Effects 0.000 claims abstract description 30
- 239000003607 modifier Substances 0.000 claims abstract description 28
- 239000002184 metal Substances 0.000 claims abstract description 22
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 10
- 239000012779 reinforcing material Substances 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 125000003368 amide group Chemical group 0.000 claims abstract description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 3
- 125000004433 nitrogen atom Chemical group N* 0.000 claims abstract description 3
- 239000000049 pigment Substances 0.000 claims description 9
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical class CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 4
- UAUDZVJPLUQNMU-UHFFFAOYSA-N Erucasaeureamid Natural products CCCCCCCCC=CCCCCCCCCCCCC(N)=O UAUDZVJPLUQNMU-UHFFFAOYSA-N 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- UAUDZVJPLUQNMU-KTKRTIGZSA-N erucamide Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(N)=O UAUDZVJPLUQNMU-KTKRTIGZSA-N 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- FUSNPOOETKRESL-ZPHPHTNESA-N (z)-n-octadecyldocos-13-enamide Chemical compound CCCCCCCCCCCCCCCCCCNC(=O)CCCCCCCCCCC\C=C/CCCCCCCC FUSNPOOETKRESL-ZPHPHTNESA-N 0.000 claims description 2
- 239000000412 dendrimer Substances 0.000 claims description 2
- 229920000736 dendritic polymer Polymers 0.000 claims description 2
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 claims description 2
- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 claims description 2
- 239000011324 bead Substances 0.000 abstract description 27
- 238000007789 sealing Methods 0.000 abstract description 24
- 230000014759 maintenance of location Effects 0.000 abstract description 5
- 238000012545 processing Methods 0.000 abstract description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 16
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 16
- 238000012360 testing method Methods 0.000 description 13
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 8
- 239000005711 Benzoic acid Substances 0.000 description 8
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 8
- 239000003963 antioxidant agent Substances 0.000 description 8
- 230000003078 antioxidant effect Effects 0.000 description 8
- 235000010233 benzoic acid Nutrition 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 239000012760 heat stabilizer Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 235000011037 adipic acid Nutrition 0.000 description 4
- 239000001361 adipic acid Substances 0.000 description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- YQLZOAVZWJBZSY-UHFFFAOYSA-N decane-1,10-diamine Chemical compound NCCCCCCCCCCN YQLZOAVZWJBZSY-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000001746 injection moulding Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 239000012466 permeate Substances 0.000 description 3
- 238000004383 yellowing Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- OYNOCRWQLLIRON-UHFFFAOYSA-N 1-n,3-n-bis(2,2,6,6-tetramethylpiperidin-4-yl)benzene-1,3-dicarboxamide Chemical compound C1C(C)(C)NC(C)(C)CC1NC(=O)C1=CC=CC(C(=O)NC2CC(C)(C)NC(C)(C)C2)=C1 OYNOCRWQLLIRON-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000004705 High-molecular-weight polyethylene Substances 0.000 description 1
- 229910000004 White lead Inorganic materials 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- OJMOMXZKOWKUTA-UHFFFAOYSA-N aluminum;borate Chemical compound [Al+3].[O-]B([O-])[O-] OJMOMXZKOWKUTA-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- 229960000892 attapulgite Drugs 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 229910001701 hydrotalcite Inorganic materials 0.000 description 1
- 229960001545 hydrotalcite Drugs 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000009916 joint effect Effects 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- DDLUSQPEQUJVOY-UHFFFAOYSA-N nonane-1,1-diamine Chemical compound CCCCCCCCC(N)N DDLUSQPEQUJVOY-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052625 palygorskite Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229910052903 pyrophyllite Inorganic materials 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 229920006114 semi-crystalline semi-aromatic polyamide Polymers 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- -1 triazine thiol Chemical class 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
-
- 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
- C08K5/20—Carboxylic acid amides
-
- 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
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
- F21V21/00—Supporting, suspending, or attaching arrangements for lighting devices; Hand grips
- F21V21/10—Pendants, arms, or standards; Fixing lighting devices to pendants, arms, or standards
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
- F21V7/00—Reflectors for light sources
- F21V7/22—Reflectors for light sources characterised by materials, surface treatments or coatings, e.g. dichroic reflectors
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Engineering & Computer Science (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a polyamide composition, a preparation method and application thereof. The polyamide composition comprises, by weight, 30-90 parts of semi-aromatic polyamide, 0-60 parts of a reinforcing material and 0.1-5 parts of a surface modifier; the semi-aromatic polyamide has a relative viscosity of 2 to 2.4; the semi-aromatic polyamide adopts ASTM D3418-2003 standard, and the crystallization temperature is measured to be more than or equal to 265 ℃ and the crystallization half-peak width is measured to be 6.5-16 ℃; the surface modifier contains amide groups and carbon chain structures, and the number of carbon atoms/the number of nitrogen atoms is more than 18. The polyamide composition disclosed by the invention has good fluidity, excellent whiteness value retention rate, good dimensional stability and processing performance, the LED reflecting support is deformed in the using process to reduce the sealing performance of the LED lamp bead, and the proper crystallization speed is provided to be combined with the surface modifier, so that the bonding performance between the polyamide composition and metal can be improved, and the sealing performance of the LED lamp bead is further improved.
Description
Technical Field
The invention relates to the technical field of high molecular compounds, and particularly relates to a polyamide composition and a preparation method and application thereof.
Background
Compared with incandescent light sources, light Emitting Diodes (LEDs) have many advantages such as low power consumption, small size, long service life, and high brightness, and have been widely used in the fields of traffic signals, daily lighting, television displays, automotive displays, and flashlights. However, the existing resin composition LED components are exposed to light and high temperature environment for a long time during the manufacturing or using process, and thus are prone to oxidation and yellowing, which affects the reflection effect of light; in addition, when the bonding performance between the LED component and the sealant and the metal is poor, a sealing structure is difficult to form, so that oxygen enters the inside of the LED in the using process, the problems of aging of the reflecting support, oxidation of a chip and the like can be caused, and the luminous effect and the service life of the LED are seriously influenced.
Therefore, in order to solve the problems of the light emitting effect and the service life of the LED, the LED reflective support material itself needs to have good long-term aging resistance, and the LED reflective support material needs to have good bonding performance with other components, especially the bonding performance with the metal component has an important influence on the sealing performance of the LED lamp bead.
For example, in the prior art, a method for producing a metal-polymer composite is disclosed, in which a triazine thiol derivative is used to form a coating film on a metal surface to increase the bonding performance between the metal and a semi-crystalline polyamide, but in the field of LEDs, the formation of the coating film on the metal surface not only increases the process cost, but also affects the heat dissipation of a chip and causes the contamination of an electrode, and thus a material having good bonding performance with a metal component is required to solve the problems of yellowing and chip oxidation of an LED reflective support due to the sealing performance.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings of yellowing and chip oxidation problems caused by sealing performance of the existing LED reflecting support, and provides a polyamide composition, which is prepared by matching semi-aromatic polyamide with specific relative viscosity, crystallinity and crystallization half-peak width with a surface modifier containing an amide group and a carbon chain structure, so that the polyamide composition has good bonding performance with metal, and the sealing performance between the polyamide composition and other parts when the polyamide composition is used as the LED reflecting support is obviously improved.
Another object of the present invention is to provide a process for the preparation of a polyamide composition.
Still another object of the present invention is to provide the use of the above polyamide composition in LED reflector panels.
It is yet another object of the present invention to provide an LED reflective support.
The above purpose of the invention is realized by the following technical scheme:
the polyamide composition comprises the following components in parts by weight:
30-90 parts of semi-aromatic polyamide;
0-60 parts of reinforcing materials;
0.1-5 parts of a surface modifier;
wherein the semi-aromatic polyamide has a relative viscosity of 2 to 2.4;
the semi-aromatic polyamide adopts ASTM D3418-2003 standard, and the crystallization temperature is measured to be more than or equal to 265 ℃ and the crystallization half-peak width is measured to be 6.5-16 ℃;
the surface modifier contains an amide group and a carbon chain structure, and the number of carbon atoms/the number of nitrogen atoms is more than 18.
According to the invention, the semi-aromatic polyamide with specific viscosity is adopted to ensure that the polyamide composition has good fluidity, so that the polyamide composition is in full contact with metal parts, and the sealing property of a product is improved. Meanwhile, the surface modifier in the composition can migrate to the surface of a product of the polyamide composition, and a smoother and smoother structure is formed on the contact interface of the product and a metal part by utilizing the carbon chain structure of the surface modifier, so that the bonding strength of the polyamide composition and the metal is improved, and the sealing property of the product is further improved.
In addition, the crystallization temperature and the crystallization half-peak width of the semi-aromatic polyamide directly influence the molding performance of the polyamide composition, and further influence the sealing performance of a product. The lower the crystallization temperature and the larger the crystallization half-peak width, the more easily a sealing structure is formed; however, if the crystallization temperature is too low, the polyamide composition is difficult to cure and form, so that the demolding is difficult, the sealing structure of the part is damaged, and the sealing property of the part is reduced; if the half-peak width of the crystal is too large, the product is deformed due to cold crystallization in the use process, the dimensional stability of the product is reduced, and the sealing property of the product is further influenced.
Specifically, the reinforcing material may be one or more of glass fiber, alumina, barium carbonate, aluminum nitride, boron nitride, potassium titanate, kaolin, clay, pyrophyllite, bentonite, calcium silicate, attapulgite, aluminum borate, calcium sulfate, barium sulfate, asbestos, glass beads, graphite, carbon nanotubes, silicon carbide, sericite, hydrotalcite, and molybdenum disulfide.
Preferably, the semi-aromatic polyamide comprises the following components in parts by weight:
45-75 parts of semi-aromatic polyamide;
25-45 parts of a reinforcing material;
0.6 to 1.2 portions of surface modifier.
Preferably, the semi-aromatic polyamide has a crystallization temperature of 270 to 273 ℃ measured by ASTM D3418-2003.
Preferably, the semi-aromatic polyamide has a crystallization half-peak width of 8-12 ℃ measured by ASTM D3418-2003 standard.
Preferably, the polyamide composition further comprises 10-60 parts of pigment in parts by weight. Specifically, the pigment may be one or more of titanium oxide, zinc sulfide, white lead, zinc sulfate, barium sulfate, calcium carbonate, and aluminum oxide. Preferably, the pigment is titanium dioxide.
In a specific embodiment, the surface modifier of the present invention may specifically be one or more of erucamide, ethylene bis stearamide derivatives, oleamide, stearyl erucamide, amide group-containing dendrimers, and low molecular weight polyamide-based hindered amine.
The polyamide composition of the invention can also comprise a flow modifier and a heat stabilizer, and the flow modifier can be a metal organic salt; the heat stabilizer may be a hindered phenol type heat stabilizer.
The invention also provides a preparation method of the polyamide composition, which comprises the following steps:
the semi-aromatic polyamide and the surface modifier are uniformly mixed and then added from a main feeding port of a double-screw extruder, the reinforcing material and the pigment are added into the double-screw extruder from a side feeding port, and then the mixture is melted, extruded and granulated at the temperature of 230-330 ℃, so that the polyamide composition is obtained.
The application of the polyamide composition in the LED lamp is also within the protection scope of the invention.
The invention also provides an LED lamp bead which comprises a reflecting support, silica gel and a metal part, wherein the reflecting support is prepared from the polyamide composition serving as a raw material.
Compared with the prior art, the invention has the beneficial effects that:
the polyamide composition disclosed by the invention adopts the semi-aromatic polyamide with specific relative viscosity, crystallization temperature and crystallization half-peak width to be matched with the surface modifier for use, the semi-aromatic polyamide with appropriate relative viscosity enables the polyamide composition to have good fluidity, and the semi-aromatic polyamide with specific crystallization half-peak width enables the polyamide composition to have good dimensional stability and processing performance, so that the LED reflection support cannot deform to reduce the sealing performance of the LED lamp bead due to cold crystallization in the using process; after the polyamide composition is combined with a surface modifier, the combination property between the polyamide composition and metal can be further improved, the sealing property of the LED lamp bead is further improved, and the whiteness value retention rate reaches 97.51% -99.52%.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the present invention is not limited to the examples in any way. The starting reagents employed in the examples of the present invention are, unless otherwise specified, those that are conventionally purchased.
1. Raw material reagent
The method is characterized by comprising the following steps of (1) self-preparing semi-aromatic polyamide, wherein the relative viscosity test method of the semi-aromatic polyamide refers to GB12006.1-89;
the specific test method comprises the following steps: the relative viscosity r of the polyamide at a concentration of 1g/dL was measured in 98% concentrated sulfuric acid at 25. + -. 0.01 ℃.
The melting point (Tm) Test of the semi-aromatic polyamides is described in ASTM D3418-2003, standard Test Method for transition Temperatures of Polymers By Differential Scanning Calorimeter;
the specific test method comprises the following steps: testing the melting point of the semi-aromatic polyamide by using a Perkin Elmer Diamond DSC analyzer; nitrogen atmosphere, the flow rate is 50mL/min; during the test, the temperature is firstly increased to 340 ℃ at 20 ℃/min, the temperature is kept at 340 ℃ for 2min, then the temperature is cooled to 50 ℃ at 20 ℃/min, the temperature is increased to 340 ℃ at 20 ℃/min, the exothermic peak temperature is the crystallization temperature Tc, the peak width of half of the exothermic peak height is the crystallization half-peak width Delta T 1/2 。
Components, melting point, relative viscosity, crystallization temperature Tc, and crystallization half-value Width DeltaT of semi-aromatic polyamide of the present invention 1/2 The data are shown in table 1:
TABLE 1
The semi-aromatic polyamides A-D can be prepared by the following preparation method:
s1, a prepolymerization stage: raising the temperature of a reaction device to 50-80 ℃, adding 10.00 parts of decamethylenediamine, 1.51 parts of hexamethylenediamine, 9.63-9.70 parts of terephthalic acid, 1.47-1.48 parts of adipic acid, 0.35-0.41 part of benzoic acid, 87.3 parts of deionized water, 0.1 percent of sodium hypophosphite with the total molar weight of 0.1 percent and 1098 antioxidant with the total molar weight of 0.2 percent in terms of molar parts in the atmosphere of nitrogen or inert gas, and stirring and mixing to obtain a polyamide salt water solution; then transferring the polyamide salt aqueous solution to a polymerization device, raising the temperature to 190-220 ℃ in the atmosphere of nitrogen or inert gas, increasing the pressure to 0.7-3.0 MPa, and reacting for 60-180 min; then keeping the pressure of the system unchanged, and obtaining a dry prepolymer through flash evaporation;
s2, solid-phase tackifying: and (3) putting the prepolymer in the S1 into a rotary drum, gradually heating to 40-60 ℃ of the rotary drum temperature lower than the melting point of the prepolymer, reacting at constant temperature for 1-4 h, stopping heating, and introducing nitrogen into the rotary drum to cool to obtain the semi-aromatic polyamide A.
The process for preparing the semi-aromatic polyamide E is substantially the same as the semi-aromatic polyamide C except that: in the prepolymerization stage, 10.00 parts of hexamethylene diamine, 7.77 parts of terephthalic acid, 1.93 parts of isophthalic acid, 0.41 part of benzoic acid, 87.3 parts of deionized water, 0.1 percent of sodium hypophosphite in total molar amount and 0.2 percent of 1098 antioxidant in total molar amount are added according to molar parts.
The process for producing the semi-aromatic polyamide F is substantially the same as the semi-aromatic polyamide C except that: in the prepolymerization stage, 10.00 parts of hexamethylene diamine, 6.77 parts of terephthalic acid, 1.93 parts of isophthalic acid, 0.97 part of adipic acid, 0.41 part of benzoic acid, 87.3 parts of deionized water, 0.1 percent of sodium hypophosphite in total molar quantity and 0.2 percent of 1098 antioxidant in total molar quantity are added according to molar parts.
The process for producing the semi-aromatic polyamide G is substantially the same as the semi-aromatic polyamide C except that: in the prepolymerization stage, 10.00 parts of decamethylenediamine, 6.14 parts of terephthalic acid, 3.68 parts of isophthalic acid, 0.41 part of benzoic acid, 87.3 parts of deionized water, 0.1 percent of sodium hypophosphite in total molar amount and 0.2 percent of 1098 antioxidant in total molar amount are added according to molar parts.
The preparation method of the semi-aromatic polyamide H is basically the same as that of the semi-aromatic polyamide A, and the difference is that: in the prepolymerization stage, 10.00 parts of nonane diamine, 9.64 parts of terephthalic acid, 0.41 part of benzoic acid, 87.3 parts of deionized water, 0.1 percent of sodium hypophosphite in total molar amount and 0.2 percent of 1098 antioxidant in total molar amount are added.
The preparation method of the semi-aromatic polyamide I is basically the same as that of the semi-aromatic polyamide A, and the difference is that: in the prepolymerization stage, 10.00 parts of hexamethylene diamine, 5.27 parts of terephthalic acid, 4.87 parts of adipic acid, 0.41 part of benzoic acid, 87.3 parts of deionized water, 0.1 percent of sodium hypophosphite in total molar amount and 0.2 percent of 1098 antioxidant in total molar amount are added according to molar parts.
The preparation method of the semi-aromatic polyamide J is basically the same as that of the semi-aromatic polyamide A, and the difference is that: in the prepolymerization stage, 10.00 parts of decamethylenediamine, 9.82 parts of terephthalic acid, 0.41 part of benzoic acid, 87.3 parts of deionized water, 0.1 percent of sodium hypophosphite in total molar amount and 0.2 percent of 1098 antioxidant in total molar amount are added according to molar parts.
The preparation method of the semi-aromatic polyamide K is basically the same as that of the semi-aromatic polyamide a, and the difference is that: in the prepolymerization stage, 10 parts of hexamethylene diamine, 2.43 parts of terephthalic acid, 7.31 parts of adipic acid, 0.29 part of benzoic acid, 87.3 parts of deionized water, 0.1 percent of sodium hypophosphite in total molar quantity and 0.2 percent of 1098 antioxidant in total molar quantity are added.
The surface modifier A is erucamide- (cis) -13-docosadienamide, and the mark: armorslip E, manufacturer: jiangxi Zhilian New materials Co., ltd;
the surface modifier B is ethylene bis stearamide, and the mark is as follows: HI-LUBE EBS-300P, manufacturer: korean cell chemical corporation;
the surface modifier C is low molecular weight polyamide-based hindered amine, and is prepared by the following steps: nylostab S-EED, manufacturer: kelain;
the surface modifier D is high molecular weight polyethylene wax, and the brand number is as follows: PED191, manufacturer: america lube, l.l.c;
the flow modifier is metal organic salt, is sold in the market, and adopts the same species in parallel experiments;
the heat stabilizer is hindered phenol heat stabilizer, is commercially available, and adopts the same type in parallel experiments;
the reinforcing material is glass fiber, and the same type is adopted in the commercial and parallel experiments;
the pigment is white pigment and titanium dioxide, and the same pigment is adopted in the commercial and parallel experiments.
2. The polyamide compositions of the examples of the invention and the comparative examples were prepared by the following preparation method:
weighing the components according to a formula, uniformly mixing the semi-aromatic polyamide and the surface modifier, adding the mixture from a main feeding port of a double-screw extruder, adding the reinforcing material and the pigment into the double-screw extruder from a measuring feeding port, and then performing melt extrusion and granulation at the temperature of 230-330 ℃ to obtain the polyamide composition;
wherein the conditions of the melt extrusion of the double-screw extruder are as follows: the temperature of the first zone is 100-160 ℃, the temperature of the second zone is 290-320 ℃, the temperature of the third zone is 300-350 ℃, the temperature of the fourth zone is 260-300 ℃, the temperature of the fifth zone is 260-300 ℃, the temperature of the sixth zone is 260-300 ℃, the temperature of the seventh zone is 260-300 ℃, the temperature of the eighth zone is 260-320 ℃, the temperature of the ninth zone is 260-330 ℃ and the rotating speed of a main engine is 50-600r/min; the length-diameter ratio of the twin-screw extruder was 48.
3. Performance testing
(1) Hunter whiteness (W) test
The Hunter whiteness (W) was measured with a Color Eye 7000A Color difference meter, wherein a sample of the polyamide composition was injection-molded and had a sample size of 60 mm. Times.60 mm. Times.1 mm.
The specific test method comprises the following steps: first, the values of L, a and b in the initial state of a sample of the polyamide composition were measured, and the value W of the initial Hunter whiteness of the polyamide composition was calculated by the following equation 1 0 (ii) a Then, the polyamide composition sample was allowed to stand at a temperature of 180 ℃ for 4 hours, and then the L, a, b values thereof were measured again, and the Hunter whiteness value W after aging of the polyamide composition was calculated by the following equation 1 t (ii) a Finally, the degree of decrease in the whiteness value was evaluated by calculating the whiteness retention ratio θ of the polyamide composition sample by the formula 2.
Formula 1: w =100-((100-L) 2 +(a) 2 +(b) 2 ) 0.5
Formula 2: θ = W 0 /W T *100％
(2) Red ink penetration test
Taking 20 LED supports prepared by adopting the polyamide composition, and carrying out silica gel encapsulation to obtain LED lamp beads, wherein the LED lamp beads are transparent; soaking the obtained LED lamp bead in detection liquid of a mixture of red ink and alcohol (the purity is 90% -98%), wherein the volume ratio of the red ink to the alcohol in the mixture of the red ink and the alcohol is 1:1; then, heating and boiling, keeping for 4 hours, taking out the LED lamp beads, observing the colors of the LED lamp beads, and marking as O, wherein no red color permeates into the interior of the lamp beads to indicate that the air tightness of the LED lamp beads is good; and at least one red color permeates into the lamp bead to indicate that the LED lamp bead is poor in air tightness and is marked as X.
(3) Dimensional stability test
Reference standard ISO 2796:1986 pretreating and testing the experimental materials according to standard, setting the test temperature at 180 deg.C and humidity at 50%, standing for 4h, measuring the average value of length, width and thickness before baking, and respectively marking as L 0 、W 0 、T 0 The average values of the length, width and thickness after baking are respectively marked as L t 、W t 、T t Then the dimensional change rates are:
σ L ＝(L t -L 0 )/L 0 *100％；
σ W ＝(W t -W 0 )/W 0* *100％；
σ t ＝(T t -T 0 )/T 0* *100％。
(4) Bond strength test
The test conditions were 23 ℃ and the tensile rate 10mm/min, determined according to ISO 527-2. The injection molding sample strip is injected in the cavity of an injection molding machine at the temperature 20 ℃ higher than the melting point, the injection molding sample strip is a weld mark mold, a 10.0mm 4.0mm 0.1mm thin sheet is embedded in the position where the weld mark is generated, the thin sheet is made of copper metal surface silver-plated material, and then the tensile strength of the sample strip is tested to evaluate the bonding strength between plastic and metal.
Examples 1 to 13
The parts by weight of each component of the polyamide compositions in examples 1 to 13 are shown in tables 2 and 3.
TABLE 2 Polyamide compositions of examples 1 to 9
TABLE 3 Polyamide compositions of examples 10 to 13
Comparative examples 1 to 9
The parts by weight of the components of the polyamide compositions of comparative examples 1 to 9 are shown in Table 4.
TABLE 4 Polyamide compositions of comparative examples 1 to 9
The results of the property test of the polyamide compositions in the respective examples and comparative examples according to the above-mentioned methods are shown in Table 5.
TABLE 5 test results of examples and comparative examples
The dimensional stability of the polyamide composition and the joint action of the polyamide composition and metal influence the sealing performance of the LED lamp beads, and oxygen entering the lamp beads influences the whiteness value of the LED reflecting support, so that the whiteness value retention rate can reflect the sealing performance of the LED lamp beads to a certain degree, and the sealing performance of the LED lamp beads is further detected by combining a red ink penetration test, and the results of examples 1 to 13 show that the whiteness value retention rate of the LED reflecting support prepared from the polyamide composition reaches 97.51% -99.52%, no red ink penetrates into the LED lamp beads, and the LED lamp beads are fully proved to have good sealing performance.
As can be seen from comparative examples 1 and 2, when the relative viscosity of the semi-aromatic polyamide is too low, the polyamide composition has poor dimensional stability and low metal bonding strength, resulting in poor sealing property of LED lamp beads and severe red ink penetration; when the relative viscosity of the semi-aromatic polyamide is too high, the fluidity of the polyamide composition is poor, and the LED lamp beads cannot form good sealing performance, so that the red ink seriously permeates.
From comparative examples 3 and 4, it can be seen that when the half-peak width of the semi-aromatic polyamide is too large, the crystallization speed of the polyamide composition is slow, the molding is difficult, the cold crystallization is severe, and the polyamide composition is easy to recrystallize after the LED lamp beads are subjected to high temperature, so that the size change is large, and the red ink permeation is severe; when the crystallization half-peak width is too small, the polyamide composition has too high crystallization speed, so that the mold filling property is too poor, and particularly, the tail end of the mold is difficult to completely wrap the metal part by the polyamide composition, so that the sealing property of the LED lamp bead is poor.
As can be seen from comparative example 6, it is difficult to effectively improve the bonding of the polyamide composition to the metal surface using the surface modifier containing only a long carbon chain structure, and thus the sealing property of the LED lamp bead cannot be effectively improved.
The above examples of the present invention are merely examples for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The polyamide composition is characterized by comprising the following components in parts by weight:
30-90 parts of semi-aromatic polyamide;
0-60 parts of a reinforcing material;
0.1-5 parts of a surface modifier;
wherein the relative viscosity of the semi-aromatic polyamide is 2 to 2.4;
the semi-aromatic polyamide adopts ASTM D3418-2003 standard, and the crystallization temperature is measured to be more than or equal to 265 ℃ and the crystallization half-peak width is measured to be 6.5-16 ℃;
the surface modifier contains amide groups and carbon chain structures, and the number of carbon atoms/the number of nitrogen atoms is more than 18.
2. The polyamide composition of claim 1, comprising the following components in parts by weight:
45-75 parts of semi-aromatic polyamide;
25-45 parts of a reinforcing material;
0.6-1.2 parts of surface modifier.
3. The polyamide composition according to claim 1, wherein the semi-aromatic polyamide has a crystallization temperature of 270 to 273 ℃ measured according to ASTM D3418-2003.
4. The polyamide composition according to claim 1 or 3, wherein the semi-aromatic polyamide has a half-value width of crystallization of 8 to 12 ℃ measured according to ASTM D3418-2003.
5. The polyamide composition of claim 1, further comprising 10 to 60 parts by weight of a pigment.
6. The polyamide composition of claim 1, wherein the surface modifier is one or more of erucamide, ethylene bis stearamide derivatives, oleamide, stearyl erucamide, amide group containing dendrimers and low molecular weight polyamido hindered amines.
7. The polyamide composition of claim 6, wherein the surface modifier is erucamide and/or ethylene bis stearamide.
8. A process for the preparation of a polyamide composition according to any one of claims 1 to 7, characterized in that it comprises the following steps:
the semi-aromatic polyamide and the surface modifier are uniformly mixed and then added from a main feeding port of a double-screw extruder, the reinforcing material and the pigment are added into the double-screw extruder from a side feeding port, and then the mixture is melted, extruded and granulated at the temperature of 230-330 ℃, so that the polyamide composition is obtained.
9. Use of a polyamide composition according to any one of claims 1 to 7 in an LED lamp.
10. An LED light source component, which comprises a reflecting bracket, silica gel and a metal part, and is characterized in that the reflecting bracket is prepared by taking the polyamide composition as the raw material according to any one of claims 1 to 7.
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