CN102367324B - Polybutylene terephthalate (PBT) composite material and preparation method thereof - Google Patents
Polybutylene terephthalate (PBT) composite material and preparation method thereof Download PDFInfo
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- CN102367324B CN102367324B CN2011101746646A CN201110174664A CN102367324B CN 102367324 B CN102367324 B CN 102367324B CN 2011101746646 A CN2011101746646 A CN 2011101746646A CN 201110174664 A CN201110174664 A CN 201110174664A CN 102367324 B CN102367324 B CN 102367324B
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- 229920001707 polybutylene terephthalate Polymers 0.000 title claims abstract description 45
- -1 Polybutylene terephthalate Polymers 0.000 title claims abstract description 24
- 239000002131 composite material Substances 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 32
- 239000011347 resin Substances 0.000 claims abstract description 32
- 239000000314 lubricant Substances 0.000 claims abstract description 16
- 239000003063 flame retardant Substances 0.000 claims abstract description 12
- 239000003365 glass fiber Substances 0.000 claims abstract description 11
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 7
- 239000011159 matrix material Substances 0.000 claims description 16
- 239000003112 inhibitor Substances 0.000 claims description 15
- 230000003647 oxidation Effects 0.000 claims description 15
- 238000007254 oxidation reaction Methods 0.000 claims description 15
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical group O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 229910001415 sodium ion Inorganic materials 0.000 claims description 10
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 9
- 238000005469 granulation Methods 0.000 claims description 9
- 230000003179 granulation Effects 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 230000000979 retarding effect Effects 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 6
- 229910052787 antimony Inorganic materials 0.000 claims description 6
- 235000006708 antioxidants Nutrition 0.000 claims description 6
- 239000004417 polycarbonate Substances 0.000 claims description 6
- 229920000515 polycarbonate Polymers 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 6
- 239000004793 Polystyrene Substances 0.000 claims description 5
- 230000003078 antioxidant effect Effects 0.000 claims description 5
- 239000003822 epoxy resin Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 229920000647 polyepoxide Polymers 0.000 claims description 5
- 229920002223 polystyrene Polymers 0.000 claims description 5
- NSBGJRFJIJFMGW-UHFFFAOYSA-N trisodium;stiborate Chemical compound [Na+].[Na+].[Na+].[O-][Sb]([O-])([O-])=O NSBGJRFJIJFMGW-UHFFFAOYSA-N 0.000 claims description 5
- 238000000354 decomposition reaction Methods 0.000 claims description 3
- 229920006226 ethylene-acrylic acid Polymers 0.000 claims description 3
- 229920006225 ethylene-methyl acrylate Polymers 0.000 claims description 3
- 229920000578 graft copolymer Polymers 0.000 claims description 3
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 3
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims 1
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 239000002667 nucleating agent Substances 0.000 abstract 2
- 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 abstract 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 abstract 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 abstract 1
- 229910052794 bromium Inorganic materials 0.000 abstract 1
- 230000002195 synergetic effect Effects 0.000 abstract 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 8
- 239000011521 glass Substances 0.000 description 7
- 238000001125 extrusion Methods 0.000 description 6
- 238000005476 soldering Methods 0.000 description 4
- 229920003182 Surlyn® Polymers 0.000 description 3
- 229920006351 engineering plastic Polymers 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 101100098709 Caenorhabditis elegans taf-1 gene Proteins 0.000 description 2
- 101100205892 Caenorhabditis elegans taf-2 gene Proteins 0.000 description 2
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 2
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 2
- 150000005690 diesters Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229920013683 Celanese Polymers 0.000 description 1
- 229920000106 Liquid crystal polymer Polymers 0.000 description 1
- 229920003189 Nylon 4,6 Polymers 0.000 description 1
- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000001175 calcium sulphate Substances 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- HQQADJVZYDDRJT-UHFFFAOYSA-N ethene;prop-1-ene Chemical group C=C.CC=C HQQADJVZYDDRJT-UHFFFAOYSA-N 0.000 description 1
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/04—Particle-shaped
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
- B29C48/875—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92561—Time, e.g. start, termination, duration or interruption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a polybutylene terephthalate (PBT) composite material and a preparation method thereof. The PBT composite material comprises: by weight, 20 to 60% of PBT resin, 10 to 30% of polybutylene naphthalate (PBN) resin, 0.3 to 1% of a nucleating agent, 5 to 15% of a bromine fire retardant, 2 to 6% of a synergetic flame retardant, 2 to 5% of a flexibilizer, 0.1 to 1% of antioxidants, 0.1 to 2% of a lubricant and 10 to 50% of glass fibers. The preparation method adopts PBN resin having a fast crystallization rate and an organic nucleating agent, can prepare the PBT composite material satisfying different high-temperature post-treatment requirements through adjustment on glass fiber content, has low costs and simple preparation processes, and is easy to be controlled.
Description
[technical field]
The present invention relates to polymeric material field, relate in particular to a kind of PBT matrix material and preparation method thereof.
[background technology]
Polybutylene terephthalate (PBT) is by a class newer thermoplast engineering plastics of U.S. Celanese company in the exploitation of 20 century 70s and suitability for industrialized production, one of five large general engineering plastic, it is heat-resisting, weather-proof good, good stability of the dimension, electrical property is good, arc resistance is good, chemical proof is extremely excellent, in wet environment, still keep various physical property (for electrical property), crystallization velocity is fast, good forming ability is widely used in the fields such as automobile, electronic apparatus, industrial machinery.
Because the high temperature soft soldering is popularized in the fields such as automobile, electronic apparatus, industrial machinery now, but the PBT fusing point is lower, almost can't bear the high temperature soft soldering, so can only select special engineering plastics in some application facet, such as polyphenylene sulfide, nylon 46, LCP etc., but these materials is expensive.
[summary of the invention]
The technical problem to be solved in the present invention provides PBT matrix material of a kind of suitable high-temperature post-treatment and preparation method thereof, and this PBT matrix material can be used for life-time service under the not high condition of temperature, but the goods that need to carry out the high temperature soft soldering in the assembling process.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is, a kind of PBT matrix material is composed of the following components by weight percentage:
PBT resin 20-60%;
PBN resin 10-30%;
Nucleator 0.3-1%;
Bromide fire retardant 5-15%;
Fire retarding synergist 2-6%;
Toughner 2-5%;
Oxidation inhibitor 0.1-1%;
Lubricant 0.1-2%;
Glass fibre 10-50%.
Described PBT resin is that kinetic viscosity is that 0.80-1.2Pa.S, fusing point are 210-230 ℃ polyethylene terephthalate.
Described PBN resin is that kinetic viscosity is that 0.65-1.0Pa.S, fusing point are 235-245 ℃ poly-how dioctyl phthalate fourth diester.
Described nucleator is ethylene-acrylic acid sodium ion polymkeric substance (E-AA-Na+), ethylene-methyl methacrylate sodium ion polymkeric substance (E-MAA-Na+) or sodium stearate.
The decomposition temperature of described described bromide fire retardant is brominated epoxy resin, TDE, brominated Polystyrene or brominated polycarbonates greater than 280 ℃.
Described fire retarding synergist is antimonous oxide, sodium antimonate or antimony peroxide.
Described is the graft copolymer of ethylene-like polymer alkene and acrylic ester monomer, comprises ethylene-methyl methacrylate butyl ester-glycidyl acrylate multipolymer, ethylene-methyl acrylate copolymer and polyethylene octene-glycidyl acrylate multipolymer.
Described oxidation inhibitor is the composite of four [3-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester primary antioxidants and tricresyl phosphite (2,4-di-t-butyl phenyl ester) auxiliary anti-oxidant; The filament diameter of described glass fibre is the 4-17 micron.Described lubricant is the ethylene bis stearamide or derivatives thereof.
Above-described PBT matrix material, composed of the following components by weight percentage:
PBT resin 20-30%;
PBN resin 16-20%;
Sodium stearate 0.5-0.7%;
Brominated polycarbonates 5-6%;
Antimony peroxide 2-3%;
Toughner 2-5%;
Oxidation inhibitor 0.1-1%;
Lubricant 0.1-2%;
Glass fibre 40-50%
A kind of technical scheme of above-mentioned PBT composite material and preparation method thereof may further comprise the steps:
A, take by weighing raw material according to above-mentioned weight percent;
B, PBT resin, PBN resin, nucleator, bromide fire retardant, fire retarding synergist, toughner, oxidation inhibitor, lubricant were mixed in moderate-speed mixers 3-7 minute;
C, the raw material that the b step is mixed are thrown in twin screw extruder and the glass fibre blending, through melt extruding granulation.Processing condition are: twin screw extruder one district's temperature is 180-260 ℃, and two district's temperature are 180-260 ℃, and three district's temperature are 180-260 ℃, and four district's temperature are 180-260 ℃, and compound time of delivery in screw rod is 1-3 minute.
The present invention has following beneficial effect:
(1) because the PBN that uses among the present invention has high crystallization rate, and added nucleator, effectively improved the shortcoming of the PBT material scarce capacity of anti-the TRANSIENT HIGH TEMPERATURE, the PBT matrix material that makes can be by high temperature aftertreatments such as the welding of tin stove and wave solderings, and the surface is without melting phenomenon;
(2) because the auxiliary agent that uses is commercially available, production cost is low;
(3) preparation process is simple, and production technique is easily controlled.
[embodiment]
Suitable high-temperature post-treatment PBT matrix material provided by the invention, its composition (weight percentage) is:
PBT resin 20-60%
PBN resin 10-30%
Nucleator 0.3-1%;
Bromide fire retardant 5-15%;
Fire retarding synergist 2-6%;
Toughner 2-5%;
Oxidation inhibitor 0.1-1%;
Lubricant 0.1-2%;
Glass fibre 10-50%.
Preparation process is as follows:
(1) takes by weighing raw material according to weight percent;
(2) PBT resin, PBN resin, nucleator, bromide fire retardant, fire retarding synergist, toughner, oxidation inhibitor, lubricant were mixed in moderate-speed mixers 3-7 minute;
(3) mixed raw material among step (2) k is thrown in twin screw extruder and the glass fibre blending, through melt extruding granulation.Manufacturing condition is: the twin screw extruder temperature is 180-260 ℃, and compound time of delivery in screw rod is 1-3 minute.Below in conjunction with specific embodiment the present invention is explained in detail:
In following examples, the kinetic viscosity of polybutylene terephthalate (PBT) is that 0.80-1.2Pa.S, fusing point are 210-230 ℃ (commercially available 1100); The kinetic viscosity of poly-how dioctyl phthalate fourth diester (PBN resin) is that 0.65-1.0Pa.S, fusing point are 235-245 ℃ (Supreme Being people changes into); Nucleator is the commercially available Aclyn 285 of ethylene-acrylic acid sodium ion polymkeric substance (E-AA-Na+), the commercially available Surlyn 8920 of ethylene-methyl methacrylate sodium ion polymkeric substance (E-MAA-Na+) or sodium stearate (commercially available); Bromide fire retardant is decomposition temperature greater than 280 ℃ bromide fire retardant, such as brominated epoxy resin, (fire retardant are commercially available) such as brominated Polystyrene or brominated polycarbonates; Fire retarding synergist is antimonous oxide (commercially available), sodium antimonate (commercially available) or antimony peroxide (commercially available); Toughner is ethylene-propylene acid butyl ester-glycidyl acrylate multipolymer (commercially available AX-8900), ethylene-methyl acrylate copolymer (commercially available 1125AC) or polyethylene octene-glycidyl acrylate multipolymer (commercially available E516); Oxidation inhibitor is four [methyl-β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester primary antioxidant (commercially available 1010) and tricresyl phosphite (2,4-di-t-butyl phenyl ester) auxiliary anti-oxidant (commercially available 168) be composite by weight 1: 1; Lubricant is ethylene bis stearamide or derivatives thereof (such as commercially available TAF); The diameter of glass fibre is 4-17 micron (commercially available megalith 534A).
Embodiment 1
By weight percentage with PBT resin 55%, PBN resin 10%, nucleator Aclyn 2850.5%, brominated epoxy resin 15%, sodium antimonate 6%, toughner AX-89002%, lubricant TAF 0.5%, oxidation inhibitor 0.2%, middling speed stirrer for mixing 5 minutes, the process melt temperature is that 180--260 ℃ of twin screw extruder extruded, and adds 10% glass in the extrusion in the middle part of screw rod, granulation.Wherein the twin screw extruder temperature is 180-260 ℃, and compound time of delivery in screw rod is 3 minutes.
Embodiment 2
By weight percentage with PBT resin 40%, PBN resin 30%, nucleator Aclyn 2851%, brominated epoxy resin 15%, sodium antimonate 6%, toughner AX-89002%, lubricant TAF 0.5%, oxidation inhibitor 0.2%, middling speed stirrer for mixing 5 minutes, the process melt temperature is that 180--260 ℃ of twin screw extruder extruded, and adds 10% glass in the extrusion in the middle part of screw rod, granulation.Wherein the twin screw extruder temperature is 180-260 ℃, and compound time of delivery in screw rod is 3 minutes.
Embodiment 3
By weight percentage with PBT resin 40%, PBN resin 10%, nucleator Surlyn 89200.4%, brominated Polystyrene 10%, antimonous oxide 4%, toughner 1125AC 5%, lubricant TAF 1%, oxidation inhibitor 0.2%, middling speed stirrer for mixing 5 minutes, the process melt temperature is that 180-260 ℃ of twin screw extruder extruded, and adds 30% glass in the extrusion in the middle part of screw rod, granulation.Wherein the twin screw extruder temperature is 180-260 ℃, and compound time of delivery in screw rod is 2 minutes.
Embodiment 4
By weight percentage with PBT resin 30%, PBN resin 20%, nucleator Surlyn 8,920 0.8%, brominated Polystyrene 10%, antimonous oxide 4%, toughner 1125AC 5%, lubricant TAF 1%, oxidation inhibitor 0.2%, middling speed stirrer for mixing 5 minutes, the process melt temperature is that 180--260 ℃ of twin screw extruder extruded, and adds 30% glass in the extrusion in the middle part of screw rod, granulation.Wherein the twin screw extruder temperature is 180-260 ℃, and compound time of delivery in screw rod is 2 minutes.
Embodiment 5
By weight percentage with PBT resin 28%, PBN resin 10%, nucleator sodium stearate 0.3%, brominated polycarbonates 5%, antimony peroxide 2%, toughner E5163%, lubricant TAF 2%, oxidation inhibitor 0.2%, middling speed stirrer for mixing 5 minutes, the process melt temperature is that 180--260 ℃ of twin screw extruder extruded, and adds 50% glass in the extrusion in the middle part of screw rod, granulation.Wherein the twin screw extruder temperature is 180-260 ℃, and compound time of delivery in screw rod is 1 minute.
Embodiment 6
By weight percentage with PBT resin 20%, PBN resin 18%, nucleator sodium stearate 0.6%, brominated polycarbonates 5%, antimony peroxide 2%, toughner E5163%, lubricant TAF 2%, oxidation inhibitor 0.2%, middling speed stirrer for mixing 5 minutes, the process melt temperature is that 180--260 ℃ of twin screw extruder extruded, and adds 50% glass in the extrusion in the middle part of screw rod, granulation.Wherein the twin screw extruder temperature is 180-260 ℃, and compound time of delivery in screw rod is 1 minute.
Cross tin stove test: (range estimation judges, the surface without melting phenomenon be considered as by)
The tin stove disposition of filling a prescription embodiment 1-6 sees the following form:
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 |
| Crossed 240 ℃ in tin stove 5 seconds | OK | OK | OK | OK | OK | OK |
| Crossed 260 ℃ in tin stove 3 seconds | NG | OK | OK | OK | OK | OK |
| Crossed 260 ℃ in tin stove 5 seconds | NG | NG | OK | OK | OK | OK |
| Crossed 260 ℃ in tin stove 10 seconds | NG | NG | NG | OK | OK | OK |
| Crossed 420 ℃ in tin stove 2 seconds | NG | NG | NG | NG | NG | OK |
(remarks: OK represents and can pass through, and NG represents and can't pass through.)
By to learning after the data analysis in the above table, the content that improves PBN, nucleator and glass all can improve the anti-TRANSIENT HIGH TEMPERATURE performance of matrix material, can be fit in various degree high-temperature post-treatment PBT matrix material according to the specific requirement preparation of product high-temperature post-treatment.
Above a kind of suitable high-temperature post-treatment PBT matrix material provided by the present invention and preparation method thereof is described in detail, used specific case herein principle of the present invention and embodiment are set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof; Simultaneously, for one of ordinary skill in the art, according to thought of the present invention, all will change in specific embodiments and applications, this description should not be construed as limitation of the present invention.
Claims (6)
1. a PBT matrix material is characterized in that, and is composed of the following components by weight percentage:
Described PBT resin is that kinetic viscosity is that 0.80-1.2Pa.S, fusing point are 210-230 ℃ polybutylene terephthalate; Described PBN resin is that kinetic viscosity is that 0.65-1.0Pa.S, fusing point are 235-245 ℃ PBN; Described nucleator is ethylene-acrylic acid sodium ion polymkeric substance, ethylene-methyl methacrylate sodium ion polymkeric substance or sodium stearate; Described toughner is the graft copolymer of ethylene-like polymer alkene and acrylic ester monomer, and above graft copolymer is selected from ethylene-methyl methacrylate butyl ester-glycidyl acrylate multipolymer, ethylene-methyl acrylate copolymer or POE grafted propylene acid glycidyl ester.
2. PBT matrix material according to claim 1 is characterized in that, the decomposition temperature of described bromide fire retardant is brominated epoxy resin, TDE, brominated Polystyrene or brominated polycarbonates greater than 280 ℃.
3. PBT matrix material according to claim 1 is characterized in that, described fire retarding synergist is antimonous oxide, sodium antimonate or antimony peroxide.
4. PBT matrix material according to claim 1 is characterized in that, described oxidation inhibitor is four [3-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester primary antioxidant and tricresyl phosphite (2,4-di-t-butyl phenyl ester) auxiliary anti-oxidant composite; The filament diameter of described glass fibre is the 4-17 micron; Described lubricant is the ethylene bis stearamide or derivatives thereof.
5. PBT matrix material according to claim 1 is characterized in that, and is composed of the following components by weight percentage:
6. a PBT composite manufacture method claimed in claim 1 is characterized in that, may further comprise the steps:
A, take by weighing raw material according to the weight percent of claim 1;
B, PBT resin, PBN resin, nucleator, bromide fire retardant, fire retarding synergist, toughner, oxidation inhibitor, lubricant were mixed in moderate-speed mixers 3-7 minute;
C, the raw material that the b step is mixed are thrown in twin screw extruder and the glass fibre blending, through melt extruding granulation; Processing condition are: twin screw extruder one district's temperature is 180-260 ℃, and two district's temperature are 180-260 ℃, and three district's temperature are 180-260 ℃, and four district's temperature are 180-260 ℃, and compound time of delivery in screw rod is 1-3 minute.
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| CN112679918B (en) * | 2020-12-14 | 2023-04-18 | 江苏金发科技新材料有限公司 | Laser-weldable PBT composition and preparation method thereof |
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| CN101225220A (en) * | 2007-12-25 | 2008-07-23 | 南通市东方实业有限公司 | Flame-retardant reinforced polybutylene terephthalate compound and production method thereof |
| CN102030972A (en) * | 2011-01-18 | 2011-04-27 | 南通市东方塑胶有限公司 | Flame retardant polyester with higher electrical property and production method thereof |
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| NL1012176C2 (en) * | 1999-05-28 | 2000-11-30 | Dsm Nv | Halogen-free fire retardant composition. |
| BRPI0607414A2 (en) * | 2005-03-03 | 2009-09-01 | Prisma Fibers Inc | flame retardant compositions |
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| CN102030972A (en) * | 2011-01-18 | 2011-04-27 | 南通市东方塑胶有限公司 | Flame retardant polyester with higher electrical property and production method thereof |
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