CN105219070A - A kind of thermoplastic resin composition and preparation method thereof and application - Google Patents
A kind of thermoplastic resin composition and preparation method thereof and application Download PDFInfo
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a kind of thermoplastic resin composition, by weight, comprise following composition: a, polyamide resin 10.5 parts-93.7 parts; B, polyketone 5 parts-89 parts; Be more than or equal to 10ppm based on the total amount of palladium element and copper in the gross weight of thermoplastic resin composition and be less than or equal to 1000ppm.The thermoplastic resin composition that the present invention prepares is owing to being more than or equal to 10ppm and be less than or equal to 1000ppm containing based on the total amount of palladium element and copper in the gross weight of thermoplastic resin composition, can give thermoplastic resin composition have catch efficiently and free radical in quenching moiety, hydroperoxide decomposition effect, to described thermoplastic resin composition, there is unexpected heat stabilization.In addition, thermoplastic resin composition of the present invention has the heatproof air aging performance and resistant to hydrolysis performance that improve than generic engineering plastics or polyketone product, and by obviously less for the carburization zone thickness of the batten section of above-mentioned thermoplastic resin composition after thermo-oxidative ageing.
Description
Technical field
The present invention relates to modified thermoplastic resin's technical field, particularly a kind of thermoplastic resin composition and preparation method thereof and application.
Background technology
Polymeric amide is owing to having excellent mechanical property, chemical-resistant, workability, heatproof air aging performance, them are made to be usually used in electronic apparatus, the motor vehicle industry harsher to operating environment requirements, wherein particularly common with the application of motor car engine periphery.And polyketone is also widely used in multiple field because having excellent resistance toheat, chemical resistance, barrier and wear resistance.The low water absorbable of polyketone, high rigidity-toughness balanced performance, high heat distortion temperature, carry out combination modification with Other Engineering plastics and have potentiality.But shortcoming is that process window is narrow, to temperature sensitive, easily degrade, and intensity under dry state and rigidity are not as traditional engineering plastics.
To have polymeric amide and polyketone through alloy modification in prior art, obtain the resin combination of the characteristic such as heatproof air aging performance, shock resistance, resistance to chemical attack, resistant to hydrolysis with improvement.As everyone knows, hydrogen bond action between polyketone and polymeric amide makes them have good consistency, but, on the α position hydrogen atom of ketone carbonyl or amide nitrogen ortho position carbon atom, hydrogen atom all has more active performance, and the free radical formed in weathering process or hydroperoxide can the aging speeds of accelerated material.
Summary of the invention
In order to overcome the deficiencies in the prior art or defect, primary and foremost purpose of the present invention is to provide a kind of obvious less thermoplastic resin composition of carburization zone thickness with the section of excellent heatproof air aging performance, resistant to hydrolysis performance and the batten after thermo-oxidative ageing.
Another object of the present invention is to provide the preparation method of above-mentioned thermoplastic resin composition.
Another object of the present invention is to provide the purposes of above-mentioned thermoplastic resin composition.
The present invention is achieved by the following technical solutions:
A kind of thermoplastic resin composition, by weight, comprises following composition:
A, polyamide resin 10.5 parts-93.7 parts;
B, polyketone 5 parts-89 parts;
Be more than or equal to 10ppm based on the total amount of palladium element and copper in the gross weight of thermoplastic resin composition and be less than or equal to 1000ppm.
Preferably, be more than or equal to 20ppm based on the total amount of palladium element and copper in the gross weight of thermoplastic resin composition and be less than or equal to 700ppm.
More preferably, be more than or equal to 50ppm based on the total amount of palladium element and copper in the gross weight of thermoplastic resin composition and be less than or equal to 500ppm.
Wherein, the composite weight ratio of described palladium element and copper is 0.01:1-1:0.01.
Wherein, the testing method of palladium constituent content: select one or more the mixing solutions in nitric acid, hydrochloric acid, hydrofluoric acid, perchloric acid, sulfuric acid, phosphoric acid etc., by decomposed sample to be measured completely and solution can keep stable after, first carry out pulverization process when testing sample particle diameter is excessive.Or the testing sample that takes a morsel is put into porcelain crucible and is added a small amount of concentrated nitric acid or the vitriol oil covers watch-glass, then low-temperature heat calcination proceeds to muffle furnace high temperature sintering, the solution more than obtained or residue are by dissolving with corresponding dilute acid soln, filter, constant volume, then uses Inductively Coupled Plasma Atomic Emission Spectrometry instrument to analyze.
The testing method of copper content: select one or more the mixing solutions in nitric acid, hydrochloric acid, hydrofluoric acid, perchloric acid, sulfuric acid, phosphoric acid etc., by decomposed sample to be measured completely and solution can keep stable after, first carry out pulverization process when testing sample particle diameter is excessive.Or the testing sample that takes a morsel is put into porcelain crucible and is added a small amount of concentrated nitric acid or the vitriol oil covers watch-glass, then low-temperature heat calcination proceeds to muffle furnace high temperature sintering, the solution more than obtained or residue are by dissolving with corresponding dilute acid soln, filter, constant volume, then uses Inductively Coupled Plasma Atomic Emission Spectrometry instrument to analyze.
The total amount of palladium element and copper is lower than 10ppm in based on the gross weight of thermoplastic resin composition, the ability that cannot realize seizure and cancellation free radical and hydroperoxide decomposition improves thermal stability, especially cannot ensure the opposing thermal-oxidative aging property of polyketone; The total amount of palladium element and copper is more than 1000ppm in based on the gross weight of thermoplastic resin composition, and the processing temperature of resin can be made to cause course of processing material breakdown higher than decomposition temperature, or causes the decay of mechanical property of resin combination.
Wherein, described polyketone is selected from containing the compound derived from olefinic comonomer repeating unit and the ketone unit derived from carbon monoxide repeating unit alternating structure; Described olefinic comonomer is selected from one or more in ethene, propylene, butylene, hexene, octene, decene, laurylene, tetradecene, hexadecylene, octadecylene; Be preferably ethene and/or propylene.
Different olefinic comonomer affects the alignment degree of segment arrangement, thus determine the mechanical property of polyketone, with propylene exemplarily, propylene content is higher, the regularity of segment is lower, the winding degree of segment is higher, and degree of crystallinity is lower, and corresponding heat-drawn wire, tensile strength and flexural strength decline.The water-intake rate of polyketone caused primarily of ketone carbonyl, and the increase of propylene content can reduce water-intake rate, has active effect for the hygroscopic property reducing composition.Another the important factor affecting polyketone mechanical property is the molecular weight of polyketone, and molecular weight increases corresponding melt flow rate (MFR) and declines, and molecular weight reduces corresponding melt flow rate (MFR) to be increased.Preferably, in order to ensure the processibility of this thermoplastic resin composition, the melt flow rate (MFR) of described polyketone (240 DEG C, 2.16Kg) elect about 5g/10min-200g/10min as, be more preferably about 5g/10min-60g/10min, if melt flow rate (MFR) is greater than 60g/10min, the poor processability of thermoplastic resin composition, if melt flow rate (MFR) is less than 5g/10min, the mechanical degradation of thermoplastic resin composition.
Wherein, described polyamide resin is formed by diamine and diprotic acid Step Condensation, or is formed by lactan ring-opening polymerization, or is formed by amino acid Step Condensation, or is formed by the copolymerize in diamine, diprotic acid, lactan, amino acid; Be selected from one or more in PA46, PA66, PA6, PA11, PA12, PA610, PA612, PA1010, PA1012, PA1212, PA4T, PA6T, PA9T, PA10T, PA6I, PAMXD6, PA6I, PA66/6, PA6/66, PA6T/6I, PA6T/66; Be preferably one or more in PA66, PA6, PA610, PA612, PA1010, PA11, PA12, PA66/6; Be more preferably PA6, PA610, PA612, PA1010.
Wherein, also comprise the weighting agent of 0-60 part, be preferably the weighting agent of 0-40 part; Described weighting agent is selected from one or more in fibrous filler, Non-fibrous weighting agent, polymer-filled agent; Described fibrous filler is selected from one or more in glass fibre, carbon fiber, organic fibre; Described Non-fibrous weighting agent is selected from one or more in aluminum oxide, carbon black, clay, zirconium phosphate, kaolin, calcium carbonate, copper, diatomite, graphite, mica, silica, titanium dioxide, zeolite, talcum, wollastonite; Described polymer-filled agent is selected from granulated glass sphere and/or glass powder.
Wherein, described weighting agent is selected from the glass fibre that diameter is 7 μm-14 μm, and described glass fibre is selected from glass chopped strands and/or long glass fiber.
Wherein, also comprise the anti-impact modifier of 0-20 part, be preferably the anti-impact modifier of 0-10 part, described anti-impact modifier is selected from ethylene-acrylate-glycidyl methacrylate trimer, ethylene-butyl acrylate copolymer, ethylene/n-butyl acrylate-glycidyl methacrylate copolymer, ethylene maleic acid anhydride copolymer, the ethylene-propylene-diene copolymer of maleic anhydride graft, the styrene-maleimide multipolymer of maleic anhydride graft, maleic anhydride modified styrene-ethylene-butylene-styrene multipolymer, the styrene-acrylonitrile copolymer of maleic anhydride graft, the acrylonitrile-butadiene-styrene copolymer of maleic anhydride graft, and one or more in their hydrogenated form.
An above-mentioned thermoplastic resin composition's preparation method, comprises the steps:
1) by polyamide resin, polyketone drying to moisture content lower than 1500ppm;
2) according to proportioning, dried polyamide resin, dried polyketone, metal fever stablizer are carried out blended, then extrude the temperature of 220 DEG C-240 DEG C through twin screw extruder, cool, the total amount of palladium element and copper is more than or equal to 10ppm and is less than or equal to the thermoplastic resin composition of 1000ppm in gross weight that granulation obtains based on thermoplastic resin composition;
Wherein, described metal fever stablizer is selected from the halide salt that transistion metal compound containing one or both in copper, palladium and/or other nontransition metal are formed; Described transistion metal compound is selected from one or more in the sulfonate of cupric and palladium, carboxylate salt, vitriol, halide salt, carbaminate and complex compound thereof, be preferably one or more in venus crystals, copper sulfate, cupric chloride, cupric bromide, cupric iodide, cuprous iodide, sulfonic acid copper, acid chloride, Palladous chloride, etheric acid palladium, palladous sulfate, two (N, N-diethylamino formic acid) two (diethylamine) palladium; The halide salt that other nontransition metal described are formed is selected from one or more in Sodium Bromide, sodium iodide, Calcium Bromide, calcium iodide, magnesium bromide, magnesium iodide, Potassium Bromide, potassiumiodide, is preferably Potassium Bromide and/or potassiumiodide.
Above-mentioned thermoplastic resin composition has excellent heatproof air aging performance, resistance to chemical corrosion, resistant to hydrolysis performance, crocking resistance, oils barrier property and outstanding rigidity-toughness balanced, can be applicable to multiple industrial circle, such as comprise engine engine cover with trolley parts such as lower component, charge air cooler, hydroecium end slot, automobile exterior door handle, wheel cover, wheel arch, driving mirror bracket, luggage carrier, automotive trim door handle, foot board, gear/transmission mechanism, backrest, safety belt buckles, industrial wiring harness ribbon and other electronic apparatus component etc.
The present invention compared with prior art, has following beneficial effect:
The thermoplastic resin composition that the present invention prepares is owing to being more than or equal to 10ppm and be less than or equal to 1000ppm containing based on the total amount of palladium element and copper in the gross weight of thermoplastic resin composition, can give thermoplastic resin composition have catch efficiently and free radical in quenching moiety, hydroperoxide decomposition effect, to described thermoplastic resin composition, there is unexpected heat stabilization.In addition, thermoplastic resin composition of the present invention has the heatproof air aging performance and resistant to hydrolysis performance that improve than generic engineering plastics or polyketone product, and by obviously less for the carburization zone thickness of the batten section of above-mentioned thermoplastic resin composition after thermo-oxidative ageing.
Embodiment
Further illustrate the present invention below by embodiment, following examples are the present invention's preferably embodiment, but embodiments of the present invention are not by the restriction of following embodiment.
The testing standard of each performance or method:
The testing method of hot air aging: according to ISO527-2/1A, by the thick test rod of the 4mm of molded and shaped preparation, width 10mm, test speed 5mm/min, tests 23 DEG C of aerial aging front and aging back draft intensity (TS) (mean value of at least 5 same compositions and shaped samples test result).Hot air aging uses thermal aging oven, and regulate temperature to be 150 DEG C and carry out, after reaching digestion time 1000h, sample takes out from ageing oven, uses aluminium foil bag heat seal after being cooled to room temperature, prevents from absorbing any moisture before evaluation mechanical property.With aging front corresponding mechanical performance compare, calculate the conservation rate of tensile strength, and represent with per-cent, be designated as aging rear TS conservation rate.
The testing method of anti-hydrolytic performance: according to ISO527-2/1A, by the thick test rod of the 4mm of molded and shaped preparation, width 10mm, test speed 5mm/min, tests before 23 DEG C of aerial alcoholysis and alcoholysis back draft intensity (TS) (mean value of at least 5 same compositions and shaped samples test result).Alcoholysis by adding the mixing solutions that glycol/water ratio is 1:1 in autoclave, add molded and shaped test rod, regulate temperature to be 130 DEG C to test, test rod is taken out after autoclave temperature being cooled to room temperature after reaching the alcoholysis time 1000h of setting, by the solvent rub on its surface, use aluminium foil bag heat seal, prevent from carrying out humidity exchange with air before evaluation mechanical property.Corresponding mechanical performance compare with before alcoholysis, calculates the conservation rate of tensile strength, and represents with per-cent, is designated as the rear TS conservation rate of hydrolysis.
Density: measure according to ASTMD792.
The testing method of carburization zone thickness: cut into slices by the thermoplastic resin composition of embodiment 1-11 and comparative example 1-8 batten after above-mentioned thermo-oxidative ageing, uses microscope (AxioVert.A1, Zeiss company) to observe and measures section carburization zone thickness.
The testing method of palladium constituent content: select one or more the mixing solutions in nitric acid, hydrochloric acid, hydrofluoric acid, perchloric acid, sulfuric acid, phosphoric acid etc., by decomposed sample to be measured completely and solution can keep stable after, first carry out pulverization process when testing sample particle diameter is excessive.Or the testing sample that takes a morsel is put into porcelain crucible and is added a small amount of concentrated nitric acid or the vitriol oil covers watch-glass, then low-temperature heat calcination proceeds to muffle furnace high temperature sintering, the solution more than obtained or residue are by dissolving with corresponding dilute acid soln, filter, constant volume, then uses Inductively Coupled Plasma Atomic Emission Spectrometry instrument to analyze.
The testing method of copper content: select one or more the mixing solutions in nitric acid, hydrochloric acid, hydrofluoric acid, perchloric acid, sulfuric acid, phosphoric acid etc., by decomposed sample to be measured completely and solution can keep stable after, first carry out pulverization process when testing sample particle diameter is excessive.Or the testing sample that takes a morsel is put into porcelain crucible and is added a small amount of concentrated nitric acid or the vitriol oil covers watch-glass, then low-temperature heat calcination proceeds to muffle furnace high temperature sintering, the solution more than obtained or residue are by dissolving with corresponding dilute acid soln, filter, constant volume, then uses Inductively Coupled Plasma Atomic Emission Spectrometry instrument to analyze.
The raw material used in the present invention, but be not limited only to following raw material:
Polyamide resin: PA61013B, originates from Yu Bu company;
Polyketone: M330A, originates from Xiao Xing group of Korea S, containing propylene co-monomer;
Glass: EC11-3.0, diameter is 10 μm, originates from Taiwan BiCheng Co., Ltd;
POE-g-MAH:493D, originates from E.I.Du Pont Company;
EPDM-g-MAH:3260, originates from LG-DOW group;
CuI, CuBr, CuCl
2, PdCl
2, PdAc, KI, KBr: originate from A Faaisha company.
embodiment 1-14 and comparative example 1-5: the preparation of thermoplastic resin composition
By polyamide resin drying to moisture content lower than 1500ppm; According to the proportioning of table 1, dried polyamide resin, polyketone, metal fever stablizer are carried out blended, then extrude the temperature of 220 DEG C-240 DEG C through twin screw extruder, cool, the total amount of palladium element and copper is more than or equal to 10ppm and is less than or equal to the thermoplastic resin composition of 1000ppm in gross weight that granulation obtains based on thermoplastic resin composition; Test the palladium constituent content of this thermoplastic resin composition, copper content, tensile strength TS, aging rear TS conservation rate, hydrolysis after TS conservation rate, density and after above-mentioned thermo-oxidative ageing batten section carburization zone thickness, test result as table 2-3 shown in.
The concrete proportioning (weight part) of table 1 embodiment 1-14 and comparative example 1-5 and test performance result thereof
Table 2
Table 3
As can be seen from table 1-3 in embodiment and comparative example relatively, the thermoplastic resin composition that the present invention prepares is owing to being more than or equal to 10ppm and be less than or equal to 1000ppm containing based on the total amount of palladium element and copper in the gross weight of thermoplastic resin composition, can give thermoplastic resin composition have catch efficiently and free radical in quenching moiety, hydroperoxide decomposition effect, to described thermoplastic resin composition, there is unexpected heat stabilization.In addition, thermoplastic resin composition of the present invention has the heatproof air aging performance and resistant to hydrolysis performance that improve than generic engineering plastics or polyketone product, and by obviously less for the carburization zone thickness of the batten section of above-mentioned thermoplastic resin composition after thermo-oxidative ageing.
Claims (10)
1. a thermoplastic resin composition, by weight, comprises following composition:
A, polyamide resin 10.5 parts-93.7 parts;
B, polyketone 5 parts-89 parts;
Be more than or equal to 10ppm based on the total amount of palladium element and copper in the gross weight of thermoplastic resin composition and be less than or equal to 1000ppm.
2. thermoplastic resin composition according to claim 1, it is characterized in that, be more than or equal to 20ppm based on the total amount of palladium element and copper in the gross weight of thermoplastic resin composition and be less than or equal to 700ppm, being preferably greater than and equaling 50ppm and be less than or equal to 500ppm.
3. thermoplastic resin composition according to claim 1 and 2, is characterized in that, the composite weight ratio of described palladium element and copper is 0.01:1-1:0.01.
4. thermoplastic resin composition according to claim 1, is characterized in that, described polyketone is selected from containing the compound derived from olefinic comonomer repeating unit and the ketone unit derived from carbon monoxide repeating unit alternating structure; Described olefinic comonomer is selected from one or more in ethene, propylene, butylene, hexene, octene, decene, laurylene, tetradecene, hexadecylene, octadecylene; Be preferably ethene and/or propylene.
5. thermoplastic resin composition according to claim 1, it is characterized in that, described polyamide resin is formed by diamine and diprotic acid Step Condensation, or formed by lactan ring-opening polymerization, or formed by amino acid Step Condensation, or formed by the copolymerize in diamine, diprotic acid, lactan, amino acid; Be selected from one or more in PA46, PA66, PA6, PA11, PA12, PA610, PA612, PA1010, PA1012, PA1212, PA4T, PA6T, PA9T, PA10T, PA6I, PAMXD6, PA6I, PA66/6, PA6/66, PA6T/6I, PA6T/66; Be preferably one or more in PA66, PA6, PA610, PA612, PA1010, PA11, PA12, PA66/6; Be more preferably PA6, PA610, PA612, PA1010.
6. the thermoplastic resin composition according to any one of claim 1-5, is characterized in that, also comprises the weighting agent of 0-60 part, is preferably the weighting agent of 0-40 part; Described weighting agent is selected from one or more in fibrous filler, Non-fibrous weighting agent, polymer-filled agent; Described fibrous filler is selected from one or more in glass fibre, carbon fiber, organic fibre; Described Non-fibrous weighting agent is selected from one or more in aluminum oxide, carbon black, clay, zirconium phosphate, kaolin, calcium carbonate, copper, diatomite, graphite, mica, silica, titanium dioxide, zeolite, talcum, wollastonite; Described polymer-filled agent is selected from granulated glass sphere and/or glass powder.
7. thermoplastic resin composition according to claim 6, is characterized in that, described weighting agent is selected from the glass fibre that diameter is 7 μm-14 μm, and described glass fibre is selected from glass chopped strands and/or long glass fiber.
8. the thermoplastic resin composition according to any one of claim 1-5, is characterized in that, also comprises the anti-impact modifier of 0-20 part, is preferably the anti-impact modifier of 0-10 part, described anti-impact modifier is selected from ethylene-acrylate-glycidyl methacrylate trimer, ethylene-butyl acrylate copolymer, ethylene/n-butyl acrylate-glycidyl methacrylate copolymer, ethylene maleic acid anhydride copolymer, the ethylene-propylene-diene copolymer of maleic anhydride graft, the styrene-maleimide multipolymer of maleic anhydride graft, maleic anhydride modified styrene-ethylene-butylene-styrene multipolymer, the styrene-acrylonitrile copolymer of maleic anhydride graft, the acrylonitrile-butadiene-styrene copolymer of maleic anhydride graft, and one or more in their hydrogenated form.
9. the preparation method of the thermoplastic resin composition as described in any one of claim 1-8, comprises the steps:
1) by polyamide resin, polyketone drying to moisture content lower than 1500ppm;
2) according to proportioning, dried polyamide resin, dried polyketone, metal fever stablizer are carried out blended, then extrude the temperature of 220 DEG C-240 DEG C through twin screw extruder, cool, the total amount of palladium element and copper is more than or equal to 10ppm and is less than or equal to the thermoplastic resin composition of 1000ppm in gross weight that granulation obtains based on thermoplastic resin composition; Wherein, described metal fever stablizer is selected from the halide salt that transistion metal compound containing one or both in copper, palladium and/or other nontransition metal are formed; Described transistion metal compound is selected from one or more in the sulfonate of cupric and palladium, carboxylate salt, vitriol, halide salt, carbaminate and complex compound thereof, be preferably one or more in venus crystals, copper sulfate, cupric chloride, cupric bromide, cupric iodide, cuprous iodide, sulfonic acid copper, acid chloride, Palladous chloride, etheric acid palladium, palladous sulfate, two (N, N-diethylamino formic acid) two (diethylamine) palladium; The halide salt that other nontransition metal described are formed is selected from one or more in Sodium Bromide, sodium iodide, Calcium Bromide, calcium iodide, magnesium bromide, magnesium iodide, Potassium Bromide, potassiumiodide, is preferably Potassium Bromide and/or potassiumiodide.
10. the thermoplastic resin composition as described in any one of claim 1-8 at engine engine cover with the application in lower component, charge air cooler, hydroecium end slot, automobile exterior door handle, wheel cover, wheel arch, driving mirror bracket, luggage carrier, automotive trim door handle, foot board, gear/transmission mechanism, backrest, safety belt buckle, industrial wiring harness ribbon, other electronic apparatus component.
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