CN110791084B - Polyamide composition and preparation method thereof - Google Patents
Polyamide composition and preparation method thereof Download PDFInfo
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- CN110791084B CN110791084B CN201910924100.6A CN201910924100A CN110791084B CN 110791084 B CN110791084 B CN 110791084B CN 201910924100 A CN201910924100 A CN 201910924100A CN 110791084 B CN110791084 B CN 110791084B
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- polyamide
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- diol
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- 239000004952 Polyamide Substances 0.000 title claims abstract description 129
- 229920002647 polyamide Polymers 0.000 title claims abstract description 129
- 239000000203 mixture Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 19
- -1 aliphatic diamine Chemical class 0.000 claims abstract description 15
- 239000000945 filler Substances 0.000 claims abstract description 13
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 12
- 125000003118 aryl group Chemical group 0.000 claims abstract description 8
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 6
- 150000004985 diamines Chemical class 0.000 claims abstract description 5
- 150000001413 amino acids Chemical class 0.000 claims abstract description 3
- 150000003951 lactams Chemical class 0.000 claims abstract description 3
- 238000002844 melting Methods 0.000 claims description 19
- 230000008018 melting Effects 0.000 claims description 19
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 8
- 229910052802 copper Inorganic materials 0.000 claims description 8
- 239000010949 copper Substances 0.000 claims description 8
- 239000012765 fibrous filler Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 229920005862 polyol Polymers 0.000 claims description 7
- 150000003077 polyols Chemical class 0.000 claims description 7
- 239000003365 glass fiber Substances 0.000 claims description 6
- 229920006012 semi-aromatic polyamide Polymers 0.000 claims description 6
- 229920000577 Nylon 6/66 Polymers 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 5
- YPFDHNVEDLHUCE-UHFFFAOYSA-N 1,3-propanediol Substances OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 claims description 4
- 229940035437 1,3-propanediol Drugs 0.000 claims description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- 229920000572 Nylon 6/12 Polymers 0.000 claims description 4
- 229920006152 PA1010 Polymers 0.000 claims description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 4
- 239000012760 heat stabilizer Substances 0.000 claims description 4
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 4
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 229920006139 poly(hexamethylene adipamide-co-hexamethylene terephthalamide) Polymers 0.000 claims description 4
- 229920000166 polytrimethylene carbonate Polymers 0.000 claims description 4
- 239000001294 propane Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000000314 lubricant Substances 0.000 claims description 3
- 239000000049 pigment Substances 0.000 claims description 3
- 150000005846 sugar alcohols Polymers 0.000 claims description 3
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 claims description 2
- ZWVMLYRJXORSEP-UHFFFAOYSA-N 1,2,6-Hexanetriol Chemical compound OCCCCC(O)CO ZWVMLYRJXORSEP-UHFFFAOYSA-N 0.000 claims description 2
- 150000000180 1,2-diols Chemical class 0.000 claims description 2
- 229940043375 1,5-pentanediol Drugs 0.000 claims description 2
- PWGJDPKCLMLPJW-UHFFFAOYSA-N 1,8-diaminooctane Chemical compound NCCCCCCCCN PWGJDPKCLMLPJW-UHFFFAOYSA-N 0.000 claims description 2
- WXSVCGWHWWPQKF-UHFFFAOYSA-N 2,3-bis(2-hydroxyethyl)cyclohexan-1-ol Chemical compound OCCC1CCCC(O)C1CCO WXSVCGWHWWPQKF-UHFFFAOYSA-N 0.000 claims description 2
- PLPYCSBZHKTQPB-UHFFFAOYSA-N 2-(2-hydroxyethoxy)hexane-1,2-diol Chemical compound CCCCC(O)(CO)OCCO PLPYCSBZHKTQPB-UHFFFAOYSA-N 0.000 claims description 2
- WUIXEIPAPIJUGW-UHFFFAOYSA-N 2-[1,1-bis(2-hydroxyphenyl)propyl]phenol Chemical compound C=1C=CC=C(O)C=1C(C=1C(=CC=CC=1)O)(CC)C1=CC=CC=C1O WUIXEIPAPIJUGW-UHFFFAOYSA-N 0.000 claims description 2
- WMYINDVYGQKYMI-UHFFFAOYSA-N 2-[2,2-bis(hydroxymethyl)butoxymethyl]-2-ethylpropane-1,3-diol Chemical compound CCC(CO)(CO)COCC(CC)(CO)CO WMYINDVYGQKYMI-UHFFFAOYSA-N 0.000 claims description 2
- SCYXIBCYTMZXAC-UHFFFAOYSA-N 2-[5,5-bis(2-hydroxyphenyl)-3-methylpentyl]phenol Chemical compound C=1C=CC=C(O)C=1C(C=1C(=CC=CC=1)O)CC(C)CCC1=CC=CC=C1O SCYXIBCYTMZXAC-UHFFFAOYSA-N 0.000 claims description 2
- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 claims description 2
- PTJWCLYPVFJWMP-UHFFFAOYSA-N 2-[[3-hydroxy-2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)COCC(CO)(CO)CO PTJWCLYPVFJWMP-UHFFFAOYSA-N 0.000 claims description 2
- RSROEZYGRKHVMN-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;oxirane Chemical compound C1CO1.CCC(CO)(CO)CO RSROEZYGRKHVMN-UHFFFAOYSA-N 0.000 claims description 2
- MQUMNTKHZXNYGW-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;propane-1,3-diol Chemical compound OCCCO.CCC(CO)(CO)CO MQUMNTKHZXNYGW-UHFFFAOYSA-N 0.000 claims description 2
- YEYKMVJDLWJFOA-UHFFFAOYSA-N 2-propoxyethanol Chemical compound CCCOCCO YEYKMVJDLWJFOA-UHFFFAOYSA-N 0.000 claims description 2
- YHXNHYKKDRMEEH-UHFFFAOYSA-N 3-(2-hydroxyethoxy)propane-1,2-diol Chemical compound OCCOCC(O)CO YHXNHYKKDRMEEH-UHFFFAOYSA-N 0.000 claims description 2
- WQYPVEKEHDLOBS-UHFFFAOYSA-N 3-(2-hydroxypropoxy)propane-1,2-diol Chemical compound CC(O)COCC(O)CO WQYPVEKEHDLOBS-UHFFFAOYSA-N 0.000 claims description 2
- BJEMXPVDXFSROA-UHFFFAOYSA-N 3-butylbenzene-1,2-diol Chemical compound CCCCC1=CC=CC(O)=C1O BJEMXPVDXFSROA-UHFFFAOYSA-N 0.000 claims description 2
- BRPSWMCDEYMRPE-UHFFFAOYSA-N 4-[1,1-bis(4-hydroxyphenyl)ethyl]phenol Chemical compound C=1C=C(O)C=CC=1C(C=1C=CC(O)=CC=1)(C)C1=CC=C(O)C=C1 BRPSWMCDEYMRPE-UHFFFAOYSA-N 0.000 claims description 2
- NOEIYOLYKBVGGI-UHFFFAOYSA-N 4-[3,3-bis(2,4-dihydroxy-3-methylphenyl)propyl]-2-methylbenzene-1,3-diol Chemical compound CC1=C(O)C=CC(CCC(C=2C(=C(C)C(O)=CC=2)O)C=2C(=C(C)C(O)=CC=2)O)=C1O NOEIYOLYKBVGGI-UHFFFAOYSA-N 0.000 claims description 2
- RAEZDADOWHBDJK-UHFFFAOYSA-N 6-(2-hydroxypropoxy)hexane-1,2-diol Chemical compound CC(O)COCCCCC(O)CO RAEZDADOWHBDJK-UHFFFAOYSA-N 0.000 claims description 2
- 239000004953 Aliphatic polyamide Substances 0.000 claims description 2
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 2
- 229920000305 Nylon 6,10 Polymers 0.000 claims description 2
- 229920000393 Nylon 6/6T Polymers 0.000 claims description 2
- ALQSHHUCVQOPAS-UHFFFAOYSA-N Pentane-1,5-diol Chemical compound OCCCCCO ALQSHHUCVQOPAS-UHFFFAOYSA-N 0.000 claims description 2
- 239000004962 Polyamide-imide Substances 0.000 claims description 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 2
- 239000007983 Tris buffer Substances 0.000 claims description 2
- FDLQZKYLHJJBHD-UHFFFAOYSA-N [3-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=CC(CN)=C1 FDLQZKYLHJJBHD-UHFFFAOYSA-N 0.000 claims description 2
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 2
- 229920003231 aliphatic polyamide Polymers 0.000 claims description 2
- 239000003963 antioxidant agent Substances 0.000 claims description 2
- 230000003078 antioxidant effect Effects 0.000 claims description 2
- 239000002216 antistatic agent Substances 0.000 claims description 2
- OWBTYPJTUOEWEK-UHFFFAOYSA-N butane-2,3-diol Chemical compound CC(O)C(C)O OWBTYPJTUOEWEK-UHFFFAOYSA-N 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- 239000013522 chelant Substances 0.000 claims description 2
- JMLPVHXESHXUSV-UHFFFAOYSA-N dodecane-1,1-diamine Chemical compound CCCCCCCCCCCC(N)N JMLPVHXESHXUSV-UHFFFAOYSA-N 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims description 2
- 239000004088 foaming agent Substances 0.000 claims description 2
- 150000004820 halides Chemical class 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 239000006082 mold release agent Substances 0.000 claims description 2
- DDLUSQPEQUJVOY-UHFFFAOYSA-N nonane-1,1-diamine Chemical compound CCCCCCCCC(N)N DDLUSQPEQUJVOY-UHFFFAOYSA-N 0.000 claims description 2
- 239000002667 nucleating agent Substances 0.000 claims description 2
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 2
- 239000004014 plasticizer Substances 0.000 claims description 2
- 229920006396 polyamide 1012 Polymers 0.000 claims description 2
- 229920002312 polyamide-imide Polymers 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical class [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 2
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 claims description 2
- XJIAZXYLMDIWLU-UHFFFAOYSA-N undecane-1,1-diamine Chemical compound CCCCCCCCCCC(N)N XJIAZXYLMDIWLU-UHFFFAOYSA-N 0.000 claims description 2
- LSXDOTMGLUJQCM-UHFFFAOYSA-M copper(i) iodide Chemical group I[Cu] LSXDOTMGLUJQCM-UHFFFAOYSA-M 0.000 claims 1
- 150000002009 diols Chemical class 0.000 claims 1
- 125000003277 amino group Chemical group 0.000 abstract description 8
- 230000009172 bursting Effects 0.000 abstract description 8
- 238000003466 welding Methods 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 6
- 238000013329 compounding Methods 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- 238000011056 performance test Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000005336 cracking Methods 0.000 description 4
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009661 fatigue test Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920006122 polyamide resin Polymers 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- XHTYQFMRBQUCPX-UHFFFAOYSA-N 1,1,3,3-tetramethoxypropane Chemical compound COC(OC)CC(OC)OC XHTYQFMRBQUCPX-UHFFFAOYSA-N 0.000 description 1
- 229920000219 Ethylene vinyl alcohol Polymers 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- MZZSDCJQCLYLLL-UHFFFAOYSA-N Secalonsaeure A Natural products COC(=O)C12OC3C(CC1=C(O)CC(C)C2O)C(=CC=C3c4ccc(O)c5C(=O)C6=C(O)CC(C)C(O)C6(Oc45)C(=O)OC)O MZZSDCJQCLYLLL-UHFFFAOYSA-N 0.000 description 1
- 235000019445 benzyl alcohol Nutrition 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- GBRBMTNGQBKBQE-UHFFFAOYSA-L copper;diiodide Chemical class I[Cu]I GBRBMTNGQBKBQE-UHFFFAOYSA-L 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009864 tensile test Methods 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
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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 invention provides a polyamide composition, which comprises the following components in parts by weight: A) 20-80 parts of at least two of polyamide I, polyamide II and polyamide III; polyamide I, polyamide II, polyamide III are derived from the following recurring units: a) 0 to 35 mole% of aromatic repeat units are derived from at least one aromatic diacid having 8 to 20 carbon atoms and at least one diamine having 4 to 20 carbon atoms; b) 65 to 100mol% of the aliphatic recurring units are derived from at least one aliphatic diacid having 6 to 20 carbon atoms and at least one aliphatic diamine having 4 to 10 carbon atoms and/or an amino acid and/or a lactam having 4 to 20 carbon atoms; the content of terminal amino groups of the polyamide I, the polyamide II and the polyamide III is more than that of terminal carboxyl groups; B) 0-35 parts of a filler. The polyamide composition has the advantages of good fatigue resistance, high bursting strength and the like.
Description
Technical Field
The invention relates to the technical field of high polymer materials, and particularly relates to a polyamide composition and a preparation method thereof.
Background
Polyamide materials are often used in the industries of electronic and electric appliances, electric tools and motor vehicles which have strict requirements on working environments due to excellent mechanical properties, chemical resistance, easy processability and fatigue creep resistance. In the field of automobile industry, polyamide materials are also widely used for interior and exterior trim parts, functional parts and structural parts. The development trend of lightweight as automobile material, more and more working of plastics also appear in part under the automobile engine cover, along with diesel engine replaces gasoline engine or turbocharged replaces mechanical supercharging, improves engine air input and combustion efficiency, requires that the engine can withstand higher pressure and temperature.
Welding is the most convenient, efficient, economical and fast method for joining metal parts, and for plastic parts, welding methods are also commonly used for welding different parts. The common welding methods are classified into hot plate welding, vibration welding, spin welding, laser welding, and the like according to the difference of heat generation methods. Both improper welding materials and welding processes can result in significant defects in the weld area, such as lack of sufficient melting, presence of cracking, excessive flash of melt, etc. The most common characteristic characterizing the quality of a weld is the weld strength (resistance to rupture (tear)). The traditional polyamide product has single component, so that the problems of insufficient molten pool, excessive flash, gas generation by pyrolysis and regional cracking cannot be solved. The problems of defects such as insufficient molten pool, zone cracking, pyrolysis gas generation and excessive melt flash not only affect the appearance of the welding, but also affect the too low tear strength of the welding zone.
Therefore, in order to improve the bursting strength, the idea is improved to solve the problem of insufficient molten pool or excessive flash, avoid the cracking of a welding area and finally obtain a product with high tearing strength.
Disclosure of Invention
The invention aims to provide a polyamide composition which has the advantages of good fatigue resistance, high bursting strength and the like.
Another object of the present invention is to provide a process for producing the above polyamide composition.
The invention is realized by the following technical scheme:
a polyamide composition comprises the following components in parts by weight:
A) 20-80 parts of at least two of polyamide I, polyamide II and polyamide III;
polyamide I, polyamide II, polyamide III are derived from the following recurring units:
a) 0 to 35 mole% of aromatic repeat units are derived from at least one aromatic diacid having 8 to 20 carbon atoms and at least one diamine having 4 to 20 carbon atoms;
b) 65 to 100mol% of the aliphatic recurring units are derived from at least one aliphatic diacid having 6 to 20 carbon atoms and at least one aliphatic diamine having 4 to 10 carbon atoms and/or an amino acid and/or a lactam having 4 to 20 carbon atoms;
wherein,
polyamide I: a fully aliphatic polyamide having a melting point in the range of 175 ℃ to 220 ℃ or a semi-aromatic polyamide having a melting point in the range of 175 ℃ to 225 ℃;
polyamide II: the melting point is 225.1 ℃ to 275 ℃ and a) is 0 mol%;
polyamide III: the melting point range is 260 ℃ to 330 ℃ and a) is not 0 mol%;
the content of terminal amino groups of the polyamide I, the polyamide II and the polyamide III is more than that of terminal carboxyl groups;
B) 0-35 parts of a filler.
The content of terminal amino groups can be determined by titration: a 2 gram quantity of polyamide was added to about 70ml of phenol and the mixture was kept under stirring and at a temperature of 40 ℃ until complete dissolution of the polyamide. The solution was then titrated at about 25 ℃ by 0.1N HCl (0.05N was also used). The carboxyl end group content was also determined using titration: a 2 gram quantity of polyamide was added to about 70ml of 90% wt benzyl alcohol and the mixture was kept under stirring and at a temperature of 40 ℃ until complete dissolution of the polyamide. The solution was then passed through 0.1N NaOH/H at about 25 deg.C2Titration with O (0.05N is also possible). If the titer at which the content of terminal amino groups is measured is higher than the content of terminal carboxyl groups, it can be determined that the content of terminal amino groups > the content of terminal carboxyl groups in the polyamide.
Generally, the end-capping treatment is not performed after the end of the polyamide reaction, or the both-side end-capping treatment is performed, which results in the content of the terminal amino group and the content of the terminal carboxyl group in the polyamide being equal. The melting point of polyamide is related to the degree of perfection of crystallization and the density of hydrogen bonds, and is almost negligible affected by the kind of end group.
The polymerization regulator can be used to adjust the content of the terminal amino group and the content of the terminal carboxyl group in the polyamide resin during the polymerization. The amount of the polymerization regulator may be adjusted depending on the method and apparatus for producing the polyamide resin, and may vary depending on the volatilization, reaction, and the like of the polymerization regulator. Specifically, the amino terminal group content and the carboxyl terminal group content were controlled by reference to 201580030197.6.
In the formulation of the present invention, the increase of the terminal amino group is advantageous in suppressing the decomposition of the polyamide material after the absorption of the laser heat, and the gas generated by the decomposition remains at the interface of the welded parts to lower the welding strength.
Preferably, A) is selected from at least one of the compound of polyamide I and polyamide II, the compound of polyamide II and polyamide III and the compound of polyamide I, polyamide II and polyamide III. In the preferred formula, polyamide II must be added, and the fatigue resistance and the bursting strength are improved.
More preferably, the polyamide II represents at least 30% of the total weight of A).
As an example, the polyamide I is at least one selected from the group consisting of PA610, PA612, PA1010, PA1012, PA1212, PA12, PA11, PA1210, PA69, PA6/66, PA6/610, PA6/612, PA6/4T, PA6/6I, PA6/6T, PA6/10T, PA6/10I, PA612/6T, PA614/6T, PA6/6I/6T, PA6/66/610, and PA1010/10T, PA11/10T, PA 11/10I.
Preferably, the polyamide I is selected from semi-aromatic polyamides with a melting point range of 175-225 ℃.
The commercially available semi-aromatic polyamide segments generally have melting points above 240 ℃ due to the high proportion of semi-aromatic units. However, by controlling the content of semi-aromatic units to be low (less than 8%, even less than 5%) and by appropriate polymerization processes to control the molecular weight distribution, semi-aromatic polyamides with melting points below 225 ℃ can be obtained. It may be 215 deg.C, 208 deg.C, 196 deg.C, 183 deg.C, etc.
As an example, the polyamide II is at least one selected from PA6, PA56, PA66 and PA 46.
The polyamide III contains 8-20 carbon atoms of aromatic diacid selected from terephthalic acid and at least one of isophthalic acid, the diamine containing 4-20 carbon atoms is selected from at least one of hexamethylenediamine, octamethylenediamine, nonanediamine, decanediamine, undecanediamine, dodecanediamine, m-xylylenediamine and p-xylylenediamine;
as an example, the polyamide III is at least one selected from the group consisting of PA66/6T, PA66/6I, PA66/6T/6I, PA66/10T, PA66/10T/10I, PA 66/12T.
0-20 parts of polyol; the polyol is at least one of dihydric alcohol, trihydric alcohol, polyol with the hydroxyl number being more than or equal to four and polymeric polyol; the dihydric alcohol is at least one selected from 1, 2-ethanediol, 1, 3-propanediol, 2, 3-butanediol, 1, 5-pentanediol, 2-dimethyl-1, 3-propanediol and polyether glycol; the trihydric alcohol is selected from glycerol, trimethylolpropane, 2, 3-di (2 '-hydroxyethyl) cyclohexane-1-ol, 1, 2, 6-hexanetriol, 1,1, 1-tri- (hydroxymethyl) ethane, 3- (2' -hydroxyethoxy) propane-1, 2-diol, 3- (2 '-hydroxypropoxy) propane-1, 2-diol, 2- (2' -hydroxyethoxy) hexane-1, 2-diol, 6- (2 '-hydroxypropoxy) hexane-1, 2-diol, 1,1, 1-tri [ (2' -hydroxyethoxy) methyl ] ethane, 1,1, 1-tri [ (2 '-hydroxypropoxy) methyl ] propane, 1,1, 1-tri (4' -hydroxyphenyl) ethane, glycerol, 2, glycerol, 2 '-hydroxyethoxy, propane, 1, 2-diol, 2' -hydroxyethoxy, 1-1, 2-diol, 1-diol, 2-hydroxy-1, 1,1, 2-hydroxy-1, 2-1, 1-tris (2-hydroxy-ethoxy) propane, 1-hydroxy-1, 1,1, 1-hydroxy-1-hydroxy-1-hydroxy-1-hydroxy-1, 1-hydroxy-1, 1-hydroxy-2-hydroxy-2-hydroxy-2-hydroxy-1, 1-hydroxy-2-hydroxy-2-hydroxy-2-diol, 1,1, 1-hydroxy-2-hydroxy-2-hydroxy-2-hydroxy-2-hydroxy-2-hydroxy, At least one of 1,1, 1-tris (hydroxyphenyl) propane, 1,1, 5-tris (hydroxyphenyl) -3-methylpentane, trimethylolpropane ethoxylate and trimethylolpropane propoxylate; the polyhydric alcohol with the hydroxyl number being more than or equal to four is selected from at least one of 1,1, 3-tri (dihydroxy-3-methylphenyl) propane, 1, 4-tri (dihydroxyphenyl) butane and ditrimethylolpropane; the polyalcohol is at least one selected from 1,1,3, 3-tetra (methoxyl) propane, pentaerythritol, dipentaerythritol, tripentaerythritol, polyvinyl alcohol with certain polymerization degree and ethylene vinyl alcohol copolymer.
The filler is at least one selected from fibrous fillers and non-fibrous fillers; the fibrous filler is selected from at least one of glass fiber, carbon fiber and organic fiber, and the non-fibrous filler is selected from at least one of granular filler and lamellar filler; preferably, the filler is selected from glass fibers with the diameter of 7-20 μm.
The invention is characterized in that the compounding of polyamide I, polyamide II and polyamide III improves the performance of a resin matrix, so that the aim of the invention can be achieved without adding glass fiber; and the purpose of adding the filler is to improve other properties.
0-10 parts of additive is also included; the additive is selected from at least one of a heat stabilizer, an antioxidant, a nucleating agent, an antistatic agent, a foaming agent, a lubricant, a plasticizer, a mold release agent and a pigment; the heat stabilizer is selected from copper-containing compounds; the copper-containing compound is selected from a compound of a halide and/or an organic chelate of monovalent and/or divalent copper and potassium halide; preferably, the copper-containing complex is selected from the group consisting of monovalent copper iodides and potassium iodide complexes.
The preparation method of the polyamide composition comprises the following steps:
1) drying all components to a moisture content of less than 1500 ppm;
2) the polyamide composition is prepared by blending the materials according to the proportion, extruding the mixture by a double-screw extruder, cooling and granulating the mixture, and has the following beneficial effects:
the invention has the following beneficial effects:
the invention provides a compounding method of three types of polyamide with amino end group content being more than carboxyl end group content: the fatigue resistance and the bursting strength of the composition can be improved by compounding the polyamide I, the polyamide II and the polyamide III in pairs and compounding the polyamide I, the polyamide II and the polyamide III; further, the preferable compound composition must contain polyamide II, so that the fatigue resistance and the bursting strength are greatly improved.
Detailed Description
The present invention is further illustrated by the following specific examples, which are, however, not intended to limit the scope of the invention.
The starting materials used in the examples and comparative examples, whether they are obtained from the homemade or commercially available sources, in particular the polyamides obtained in patent reference 201580030197.6:
polyamide I: PA6/66, melting point 205 ℃;
polyamide I: PA6/10T, 10T content about 20mol%, melting point 215 ℃;
polyamide II: PA6, melting point 228 ℃;
polyamide II: PA66, melting point 263 deg.C;
polyamide III: PA66/10T, 10T content about 26mol%, melting point 310 ℃;
glass fiber: EC11-3.0, diameter 10um, produced by Taiwan Arbitrary corporation of China;
lubricant: n-octadecyl-13-docosanamide, available from helofeng;
black pigment A: carbon black, hilblack 600L, available from Orion;
black pigment B: nigrosine, L0080, available from basf;
examples and comparative examples preparation of polyamide compositions: drying all the components according to the mixture ratio of the table 1 until the moisture content is less than 1500 ppm; and blending the dried polyamide, the filler and the additive according to the proportion, and then extruding, cooling and granulating the mixture by a double-screw extruder to obtain the polyamide composition.
The performance test method comprises the following steps:
(1) and (3) fatigue resistance performance test: the MTS fatigue testing machine is used, ISO527 splines are used as fatigue testing samples, 90MPa is selected as a maximum load value, the stress ratio =0, namely the minimum load is 0, the load applied to the cross section area of the samples changes in a sine wave mode from the average load-the maximum load-the average load-the minimum load-the average load, the frequency is 3Hz, the number of times of fracture of the testing samples under the condition is determined, and the higher the number of times, the better the fatigue resistance of the material is determined.
(2) And (3) anti-explosion strength:
the composition was molded into 4X 10X 60mm cubic specimens and friction welded as upper and lower bodies, which were welded, and the specimens were wrapped with aluminum foil bags before being spread for friction welding to prevent moisture absorption in ambient storage. When the welding is carried out, the sample strips are respectively arranged on an upper clamp and a lower clamp, and the welding process comprises the steps of fixing the welding depth to be 1.2mm, fixing the amplitude to be 0.4mm and fixing the frequency to be 233.1 Hz. For the welded bars, aluminum foil wrap was also used to prevent moisture absorption before testing and to prevent loss of tear strength. For the tear strength test, a universal testing machine is adopted to carry out a tensile test, the speed of a cross beam is 5mm/min, the span of a clamp is 45mm, the welding area is positioned in the middle of the span, the measured result, unit MPa, is recorded, and the mean value of the results of 5 times of parallel tests is taken as the tear strength of the composition.
Table 1: EXAMPLES 1 to 7 respective component ratios (parts by weight) and respective results of performance tests
As can be seen from examples 3 and 4, the preferred polyamide I formulation has better fatigue resistance and bursting strength.
As can be seen from examples 1 to 7, when polyamide II is added, the fatigue resistance and the bursting strength are good; in detail, the compounding effect of polyamide I, polyamide II and polyamide III is best; the compounding of the polyamide II and the polyamide III is slightly better than that of the polyamide I and the polyamide II; although the combination of the polyamide I and the polyamide III is greatly improved compared with the single use, the effect is slightly poor compared with other combinations.
It can be seen from examples 2 and 8 that, further, when the amount of polyamide II is at least 30% of the total amount of polyamide, the improvement of the fatigue resistance and the burst strength is large.
Table 2: example 8 and comparative examples 1 to 4 each component ratio (parts by weight) and each performance test result
Table 3: comparative examples 5 to 9 composition ratios (parts by weight) and results of performance tests
As can be seen from comparative examples 1 to 4 and examples 1 to 3, the polyamide has an amino terminal group content < carboxyl terminal group content, and the decrease in the burst strength is large; when both the polyamide II and the polyamide III have an amino end group content < a carboxyl end group content, the fatigue resistance times and the burst strength are reduced considerably at the same time.
As can be seen from comparative examples 5 to 9, the above polyamide alone had poor burst strength.
Claims (11)
1. The polyamide composition is characterized by comprising the following components in parts by weight:
A) 20-80 parts of at least two of polyamide I, polyamide II and polyamide III;
polyamide I, polyamide II, polyamide III are derived from the following recurring units:
a) 0 to 35 mole% of aromatic repeat units are derived from at least one aromatic diacid having 8 to 20 carbon atoms and at least one diamine having 4 to 20 carbon atoms;
b) 65 to 100mol% of the aliphatic recurring units are derived from at least one aliphatic diacid having 6 to 20 carbon atoms and at least one aliphatic diamine having 4 to 10 carbon atoms and/or an amino acid and/or a lactam having 4 to 20 carbon atoms;
wherein,
polyamide I: a fully aliphatic polyamide having a melting point in the range of 175 ℃ to 220 ℃ or a semi-aromatic polyamide having a melting point in the range of 175 ℃ to 225 ℃;
polyamide II: the melting point is 225.1 ℃ to 275 ℃ and a) is 0 mol%;
polyamide III: the melting point range is 260 ℃ to 330 ℃ and a) is not 0 mol%;
the amino end group content of the polyamide I, the polyamide II and the polyamide III is more than the carboxyl end group content;
B) 0-35 parts of a filler;
the polyamide I is selected from at least one of PA610, PA612, PA1010, PA1012, PA1212, PA12, PA11, PA1210, PA69, PA6/66, PA6/610, PA6/612, PA6/4T, PA6/6I, PA6/6T, PA6/10T, PA6/10I, PA612/6T, PA614/6T, PA6/6I/6T, PA6/66/610 and PA1010/10T, PA11/10T, PA 11/10I;
the polyamide II is selected from at least one of PA6, PA56, PA66 and PA 46;
the polyamide III contains 8-20 carbon atoms of aromatic diacid selected from terephthalic acid and at least one of isophthalic acid, and the diamine containing 4-20 carbon atoms selected from at least one of hexamethylenediamine, octamethylenediamine, nonanediamine, decanediamine, undecanediamine, dodecanediamine, m-xylylenediamine and p-xylylenediamine.
2. The polyamide composition as claimed in claim 1, wherein A) is at least one selected from the group consisting of a combination of polyamide I and polyamide II, a combination of polyamide II and polyamide III, and a combination of polyamide I, polyamide II and polyamide III.
3. The polyamide composition as claimed in claim 2, wherein the polyamide II is at least 30% by weight of the total weight of A).
4. The polyamide composition as claimed in claim 1, wherein the polyamide I is selected from semi-aromatic polyamides having a melting point in the range of 175 ℃ to 225 ℃.
5. Polyamide composition according to claim 1, characterized in that polyamide III is selected from at least one of the group consisting of PA66/6T, PA66/6I, PA66/6T/6I, PA66/10T, PA66/10T/10I, PA 66/12T.
6. The polyamide composition of claim 1, further comprising 0 to 20 parts by weight of a polyol; the polyol is at least one selected from dihydric alcohol, trihydric alcohol and polyol with the hydroxyl number being more than or equal to four; the dihydric alcohol is at least one selected from 1, 2-ethanediol, 1, 3-propanediol, 2, 3-butanediol, 1, 5-pentanediol, 2-dimethyl-1, 3-propanediol and polyether diol; the trihydric alcohol is selected from glycerol, trimethylolpropane, 2, 3-di (2 '-hydroxyethyl) cyclohexane-1-ol, 1, 2, 6-hexanetriol, 1,1, 1-tri- (hydroxymethyl) ethane, 3- (2' -hydroxyethoxy) propane-1, 2-diol, 3- (2 '-hydroxypropoxy) propane-1, 2-diol, 2- (2' -hydroxyethoxy) hexane-1, 2-diol, 6- (2 '-hydroxypropoxy) hexane-1, 2-diol, 1,1, 1-tri [ (2' -hydroxyethoxy) methyl ] ethane, 1,1, 1-tri [ (2 '-hydroxypropoxy) methyl ] propane, 1,1, 1-tri (4' -hydroxyphenyl) ethane, glycerol, 2, glycerol, 2 '-hydroxyethoxy, propane, 1, 2-diol, 2' -hydroxyethoxy, 1-1, 2-diol, 1-diol, 2-hydroxy-1, 1,1, 2-hydroxy-1, 2-1, 1-tris (2-hydroxy-ethoxy) propane, 1-hydroxy-1, 1,1, 1-hydroxy-1-hydroxy-1-hydroxy-1-hydroxy-1, 1-hydroxy-1, 1-hydroxy-2-hydroxy-2-hydroxy-2-hydroxy-1, 1-hydroxy-2-hydroxy-2-hydroxy-2-diol, 1,1, 1-hydroxy-2-hydroxy-2-hydroxy-2-hydroxy-2-hydroxy-2-hydroxy, At least one of 1,1, 1-tris (hydroxyphenyl) propane, 1,1, 5-tris (hydroxyphenyl) -3-methylpentane, trimethylolpropane ethoxylate and trimethylolpropane propoxylate; the polyhydric alcohol with the hydroxyl number being more than or equal to four is at least one selected from 1,1, 3-tri (dihydroxy-3-methylphenyl) propane, 1, 4-tri (dihydroxyphenyl) butane, di (trimethylolpropane), pentaerythritol, dipentaerythritol and tripentaerythritol.
7. The polyamide composition according to claim 1, wherein the filler is at least one selected from the group consisting of fibrous fillers and non-fibrous fillers; the fibrous filler is at least one selected from glass fiber, carbon fiber and organic fiber, and the non-fibrous filler is at least one selected from granular filler and lamellar filler.
8. Polyamide composition according to claim 7, characterized in that the filler is chosen from glass fibres having a diameter of from 7 μm to 20 μm.
9. The polyamide composition of claim 1, further comprising 0 to 10 parts by weight of an additive; the additive is selected from at least one of a heat stabilizer, an antioxidant, a nucleating agent, an antistatic agent, a foaming agent, a lubricant, a plasticizer, a mold release agent and a pigment; the heat stabilizer is selected from copper-containing compounds; the copper-containing complex is selected from the complex of a halide and/or an organic chelate of monovalent and/or divalent copper and a potassium halide.
10. Polyamide composition according to claim 9, characterized in that the copper-containing complex is selected from the group consisting of copper monoiodide and potassium iodide complexes.
11. Process for the preparation of a polyamide composition according to any one of claims 1 to 10, characterized in that it comprises the following steps:
1) drying all components to a moisture content of less than 1500 ppm;
2) the materials are blended according to the proportion, and then are extruded, cooled and granulated by a double-screw extruder to obtain the polyamide composition.
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