CN104004338A - Anti-hydrolysis anti-static PC/ASA alloy and preparation method thereof - Google Patents
Anti-hydrolysis anti-static PC/ASA alloy and preparation method thereof Download PDFInfo
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Abstract
The invention provides anti-hydrolysis anti-static PC/ASA alloy and a preparation method thereof. According to the method, condensation polymerization is conducted on PPR-MWCNT compounds and ASA-g-MAH grafted copolymer through bisphenol A and epoxy chloropropane, bisphenol A epoxy resin (EP-E51) and polycarbonate (PC) are obtained and are subjected to blending extrusion, and the anti-hydrolysis anti-static PC/ASA alloy is obtained. The prepared anti-hydrolysis anti-static PC/ASA alloy has excellent anti-static performance and excellent hydrolysis resistance, is suitable for the moist rainwater weather, has excellent impact toughness and lower processing viscosity, is easy to process and suitable for mass production and popularization, and can be oriented to automobile inside and outside ornaments such as an automobile rearview mirror shell body and an automobile door plank and outdoor sport equipment.
Description
Technical field
What the present invention relates to is a kind of method of technical field of polymer materials, specifically a kind of hydrolysis anti-static polycarbonate (PC)/Bing Xi Jing ?Ben Yi Xi ?acrylate graft copolymers (ASA) Alloy And Preparation Method.
Background technology
The rubbery kernel strata acrylic elastomer of ASA graft copolymer is saturated structures, not containing residual double bonds, under the high energy gamma source light of the following wavelength of 300nm, dissociate, in tellurian solar ray, there is not this high energy gamma source light, the molecular structure that is ASA resin is difficult for by high energy gamma source photolysis, and PC/ASA has high weathering resistance.PC/ASA alloy is PC and ASA premium properties separately comprehensively, improves thermotolerance, shock resistance and the tensile strength of ASA, reduces PC melt viscosity, improves processing characteristics, reduces goods internal stress, significantly improves the outdoor weatherability of PC.
Affect plastic degradation Wu Li ?chemical factor more, have heat, mechanical force, ultrasonic wave, light, oxygen, water, pharmaceutical chemicals, microorganism etc.Under moist, warm environment, water molecules destroys the macromole long-chain that forms polymkeric substance, causes polymkeric substance to degrade at leisure even losing the phenomenon of any performance to be called hydrolysis.Hydrocarbon polymer is more stable to moisture, but polycarbonate (PC) and Bing Xi Jing ?Ben Yi Xi ?acrylate graft copolymers (ASA) contain the high polar group of a large amount of ester groups, when the higher and relative humidity of temperature is larger, the polar group of water and polymer molecular chain reacts and causes degraded.The PC/ASA alloy that hydrolysis occurs can losing property antistatic property, even causes colour-change, mechanical property degradation.Meanwhile, for exterior trimming parts such as automobiles, also require static resistance, avoid adsorbing a large amount of dusts and affect gadget effect.
Through the retrieval of prior art is found, Chinese patent literature CN103740081A open (bulletin) day 2014.04.23, a kind of low smell, high-impact PC/ASA intermingling material and preparation method thereof are disclosed, the raw material that comprises following weight percent meter: polycarbonate (PC): 20 ?80%, Bing Xi Qing ?phenylethene grafted copolymer: 10 ?55%, Bing Xi Jing ?Ben Yi Xi ?acrylate graft copolymers ASA:5 ?35%, compatilizer: 2 ?15%, deodovization agent: 0.2 ?2%.Raw material through mixing is placed in to screw diameter 35mm, length-to-diameter ratio L/D=36 is in twin screw extruder main barrel, main barrel exports minute nine sections of control temperature from charging opening to head, be followed successively by 200 ℃, 230 ℃, 255 ℃, 255 ℃, 255 ℃, 255 ℃, 255 ℃, 255 ℃, 240 ℃, twin screw rotating speed is 300 revs/min, extrudes material strip pelletizing after tank is cooling and obtains product.The automotive upholstery goods that the PC/ASA intermingling material being obtained by this technical scheme is made, have low smell, high-impact, and the advantages such as good weatherability can be widely used in automotive upholstery, as sun visor, fascia etc.But defect and the deficiency of this technology are: these materials can not be exposed to hot and humid environment and be applied as exterior trimming parts, do not have static resistance can resist the erosion of exterior trim ambient dust simultaneously.
Chinese patent literature CN103709712A open (bulletin) day 2014.04.09, a kind of heat-resisting hydrolysis PC/ASA alloy material is disclosed, belong to technical field of polymer materials, comprise the following component according to parts by weight meter: 80～100 parts of polycarbonate, Bing Xi Jing ?Ben Yi Xi ?20～50 parts of acrylate graft copolymers, 6～10 parts, carbon fiber, Ben Yi Xi ?4～9 parts of maleic anhydride graft copolymers, 1～3 part of polycarbodiimide, 6221～4 parts of photostabilizers, 0.5～3 part, oxidation inhibitor, 1.2～3.5 parts of lubricants.This technology adopt Bing Xi Jing ?Ben Yi Xi ?acrylate graft copolymers, it is ASA resin, with PC plastic blend, and added carbon fiber and Ben Yi Xi ?maleic anhydride graft copolymer strengthen, make that PC/ASA alloy material heat resisting temperature after blend is high, weather resistance is excellent, shock resistance is good, meanwhile, there is good anti-hydrolytic performance and processing characteristics.But defect and the deficiency of this technology are: this kind of material do not have static resistance during as exterior trimming parts, can not resist the erosion of exterior trim ambient dust, cannot prolonged application in exterior trim environment, be unfavorable for this kind of material large-scale promotion and application.
Summary of the invention
The present invention is directed to prior art above shortcomings, propose a kind of polycarbonate/Bing Xi Jing ?Ben Yi Xi ?acrylate graft copolymers Alloy And Preparation Method, by add self-control epoxy resin EP ?E51, epoxy addition reaction can catch the carboxyl that polymkeric substance hydrolysis produces effectively, harmless product is stablized in generation, stop polymkeric substance to be further hydrolyzed, thereby make PC/ASA alloy material there is superelevation hydrolytic resistance and good static resistance; Because alloy contains Co-polypropylene (PPR), PPR has flexibility and makes alloy material have good impact property and good processing characteristics simultaneously; ASA ?g ?MAH make alloy there is good consistency.
The present invention is achieved by the following technical solutions: the present invention by respectively by atactic copolymerized polypropene (PPR) and multi-walled carbon nano-tubes (MWCNT) melt blending, by Bing Xi Jing ?Ben Yi Xi ?phenylethene grafted copolymer (ASA) and maleic anhydride (MAH) melt blending, extrude separately pelletizing obtain PPR ?MWCNT mixture and ASA ?g ?MAH graft copolymer; With dihydroxyphenyl propane and epoxy chloropropane, by polycondensation, make bisphenol A type epoxy resin (EP ?E51) in addition, then by polycarbonate (PC), ASA ?g ?MAH, PPR ?MWCNT, EP ?E51 blending extrusion obtain polycarbonate/Bing Xi Jing ?Ben Yi Xi ?phenylethene copolymer alloy.
Described blending extrusion refers to: by PC, ASA ?g ?MAH, PPR ?MWCNT, EP ?E51 and auxiliary agent melt blending to squeeze temperature be 200～250 ℃, screw speed is 200～300r/min.
Described PC, ASA ?g ?MAH, PPR ?MWCNT, EP ?the weight ratio of E51 and auxiliary agent be: PC40 ?80 parts, ASA ?g ?MAH20 ?60 parts, PPR ?MWCNT5 ?20 parts, EP ?E511 ?10 parts, auxiliary agent 0.5 ?5 parts.
Described auxiliary agent comprises: oxidation inhibitor, thermo-stabilizer, lubricant, anti ultraviolet agent; Its weight ratio is: oxidation inhibitor 0.1 ?1 part, thermo-stabilizer 0.1 ?1 part, lubricant 0.1 ?1 part, anti ultraviolet agent 0.2 ?2 parts.
By dihydroxyphenyl propane and epoxy chloropropane, polycondensation under base catalysis condition forms described bisphenol A type epoxy resin, wherein: dihydroxyphenyl propane and epoxy chloropropane mol ratio are (n+1): (n+2), in embodiment, n value is 80～100, and oxirane value is 0.48～0.54mol/100g; The equation of this polycondensation is:
Described ASA ?g ?MAH by the reaction of ASA and MAH melt blending, extrude and make, adopt dicumyl peroxide (DCP) as catalyzer, melt blending extrusion temperature is 180～200 ℃, screw speed is 150～250r/min; Percentage of grafting is 5～15%.
Described ASA and the weight ratio of MAH are (70～80): (20～30).
Described PPR ?MWCNT by PPR and MWCNT melt blending, extrude and make, melt blending extrusion temperature is 200～220 ℃, screw speed is 200～250r/min.
Described PPR and the weight ratio of MWCNT are (70～95): (5～30).
Described first melt blending extrude pelletizing obtain PPR ?MWCNT particle, then by PPR ?MWCNT particle and PC, ASA ?g ?the melt blending such as MAH prepare PC/ASA alloy material, this preparation method has solved MWCNT scattering problem in PC/ASA alloy material, and it is uniformly dispersed.
Described maleic anhydride (MAH) is colourless acicular crystal, and by infrared spectrum characterization, acid anhydrides charateristic avsorption band is at 1778.68cm
-1place.
Described atactic copolymerized polypropene (PPR) adopts the RP2400 of Kpic.
The epoch nanometer M1205 of section during described multi-walled carbon nano-tubes (MWCNT) adopts, mean length be 10 ?30 μ m, mean diameter 20 ?30nm.
Described oxidation inhibitor is one or more in Hinered phenols antioxidant and phosphite ester kind antioxidant, is preferably Hinered phenols antioxidant 1010, i.e. four [first base ?β ?(the tertiary Ding Ji ?4 ?hydroxy phenyls of 3,5 ?bis-) propionic ester] tetramethylolmethane.
Described lubricant be fatty acid ester or oxidized polyethlene wax one or more, preferably use pentaerythritol stearate (PETS).
Described anti ultraviolet agent is one or more of benzotriazole category, triazines, benzophenone, hindered amines, preferably benzotriazole category light absorber.
Described thermo-stabilizer be organic tin thermo-stabilizer, metal soap thermal stabilizers one or more, preferred toxilic acid pink salt organo-tin het stabilizer.
The socle girder notched Izod impact strength of described PC/ASA alloy material is greater than 650J/m under 23 ℃ of environment, and surface resistivity reaches 10
9ohm, reaches 10 through 90 ℃, 96RH% fixed temperature and humidity 24h hydrolysis reaction rear surface resistance
9ohm, there is not being hydrolyzed phenomenon in material.
The present invention relates to above-mentioned polycarbonate/Bing Xi Jing ?Ben Yi Xi ?the application of acrylate alloy, use it for inner and outer decorative parts of automobile such as preparing automobile rearview mirror, door panel, can be used for other outdoor activity sports equipment goods simultaneously.
Embodiment
Below embodiments of the invention are elaborated, the present embodiment is implemented take technical solution of the present invention under prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The present embodiment comprises the following steps:
1) the bisphenol A polycarbonate PC lexan141R of the polycarbonate WeiGE company that following examples are used, molecular weight is 25000 ?28000g/mol.Bing Xi Jing ?Ben Yi Xi ?acrylate graft copolymers be the strange beautiful PW957 in Taiwan, by weight percentage acrylic elastomer content be 40 ?80%.Oxidation inhibitor is used four [β ?(the special fourth base of 3,5 ?bis-?4 ?hydroxy phenyls) propionic acid] pentaerythritol ester, and commodity are called Irganox1010, and Ciba fine chemicals produces.The present invention use ZE that German Berstorff company produces ?25 twin screw extruders.
The present embodiment comprises the following steps:
1) grafting ASA ?g ?the preparation of MAH:
First 80 parts of ASA, 20 parts of MAH, 1.5 parts of dicumyl peroxides (DCP), 0.1 part of Hinered phenols antioxidant 1010 use high-speed mixer are evenly mixed to join after 5 minutes and in twin screw extruder, carry out melt blending, one district's temperature is 180 ℃, two district's temperature are 185 ℃, three district's temperature are 190 ℃, four district's temperature are 190 ℃, five district's temperature are 195 ℃, six district's temperature are 195 ℃, seven district's temperature are 200 ℃, eight district's temperature are 200 ℃, nine district's temperature are 195 ℃, and screw speed is 200 revs/min, the residence time be 1 ?3 minutes.Cooling after extruding, dry, pelletizing, obtain ASA ?g ?MAH graft copolymer;
2) PPR ?the preparation of MWCNT mixture:
90 parts of PPR, 10 parts of MWCNT, 0.1 part of Hinered phenols antioxidant 1010 use high-speed mixer are evenly mixed to join after 5 minutes and in twin screw extruder, carry out melt blending, one district's temperature is 200 ℃, two district's temperature are 200 ℃, three district's temperature are 205 ℃, four district's temperature are 205 ℃, five district's temperature are 210 ℃, six district's temperature are 210 ℃, seven district's temperature are 215 ℃, and eight district's temperature are 220 ℃, and nine district's temperature are 215 ℃, screw speed is 200 revs/min, the residence time be 1 ?3 minutes, through cooling, dry, pelletizing, obtain PPR ?MWCNT mixture.
3) polycarbonate/Bing Xi Jing ?Ben Yi Xi ?the preparation of acrylate copolymer alloy
By PC, ASA ?g ?MAH, EP ?E51, PPR ?MWCNT, Hinered phenols antioxidant, thermo-stabilizer, lubricant and anti ultraviolet agent evenly mix to join after 10 minutes with high-speed mixer according to the weight proportion of embodiment and in twin screw extruder, carry out melt blending, one district's temperature is 200 ℃, two district's temperature are 210 ℃, three district's temperature are 220 ℃, four district's temperature are 230 ℃, five district's temperature are 240 ℃, six district's temperature are 240 ℃, seven district's temperature are 250 ℃, eight district's temperature are 250 ℃, nine district's temperature are 245 ℃, screw speed is 250 revs/min, the residence time is 2 minutes.Cooling after extruding, dry, pelletizing, obtain PC/ASA alloy.
Notched Izod impact strength is tested by ASTM D256, and specimen size is 64mm*12.7mm*3.2mm, and notch depth is 2.2mm, testing apparatus be Britain Ray ?the shock-testing machine of Ran company.
IEC60093 is pressed in surface resistivity test, testing apparatus be U.S. ACL ?800 surface resistivity instrument.
Each weight percent and test physical property result are as following table:
Table 1
In embodiment, add self-control Co-polypropylene and multi-walled carbon nano-tubes mixture PPR ?after MWCNT, make polycarbonate/Bing Xi Jing ?Ben Yi Xi ?acrylate copolymer (PC/ASA) alloy material there is good static resistance, and with PPR ?MWCNT content to increase static resistance better, surface resistivity arrives 10
9ohm.
In embodiment, add self-control PPR ?after MWCNT mixture, because PC/ASA alloy material contains flexible PPR, make alloy material there is higher notch impact toughness, normal temperature notched Izod impact strength with PPR ?MWCNT content increase.
In embodiment, add epoxy resin EP ?after E51, make PC/ASA alloy material there is superelevation hydrolytic resistance, through after 90 ℃, 96RH% fixed temperature and humidity 24h, there is not hydrolysis phenomenon in alloy material, surface resistivity reaches 10 equally
9ohm.
Claims (10)
1. the preparation method of a polycarbonate/the third alkene nitrile ?benzene second alkene ?acrylate graft copolymers alloy, it is characterized in that, by respectively by PPR and MWCNT melt blending, by ASA and MAH melt blending, extrude separately pelletizing obtain PPR ?MWCNT mixture and ASA ?g ?MAH graft copolymer; In addition with dihydroxyphenyl propane and epoxy chloropropane by polycondensation make EP ?E51, then by PC, ASA ?g ?MAH, PPR ?MWCNT, EP ?E51 blending extrusion obtain polycarbonate/Bing Xi Jing ?Ben Yi Xi ?phenylethene copolymer alloy;
In described blending extrusion PC, ASA ?g ?MAH, PPR ?MWCNT, EP ?the weight ratio of E51 be: PC40 ?80 parts, ASA ?g ?MAH20 ?60 parts, PPR ?MWCNT5 ?20 parts, EP ?E511 ?10 parts.
2. method according to claim 1, it is characterized in that, described blending extrusion refers to: by PC, ASA ?g ?MAH, PPR ?MWCNT, EP ?E51 and auxiliary agent melt blending, wherein: PC, ASA ?g ?MAH, PPR ?MWCNT, EP ?the weight ratio of E51 be: PC60 ?80 parts, ASA ?g ?MAH20 ?40 parts, PPR ?MWCNT5 ?20 parts, EP ?E515 ?10 parts, auxiliary agent 0.5 ?5 parts.
3. method according to claim 2, is characterized in that, described auxiliary agent comprises: oxidation inhibitor, thermo-stabilizer, lubricant, anti ultraviolet agent; Its weight ratio is: oxidation inhibitor 0.1 ?1 part, thermo-stabilizer 0.1 ?1 part, lubricant 0.1 ?1 part, anti ultraviolet agent 0.2 ?2 parts.
4. method according to claim 1, it is characterized in that, by dihydroxyphenyl propane and epoxy chloropropane, polycondensation under base catalysis condition forms described bisphenol A type epoxy resin, wherein: dihydroxyphenyl propane and epoxy chloropropane mol ratio are (n+1): (n+2), n be 80 ?100, oxirane value is 0.48～0.54mol/100g; The equation of this polycondensation is:
。
5. method according to claim 1, it is characterized in that, described ASA ?g ?MAH by the reaction of ASA and MAH melt blending, extrude and make, adopt dicumyl peroxide as catalyzer, melt blending extrusion temperature is 180～200 ℃, and screw speed is 150～250r/min; Percentage of grafting is 5～15%.
6. method according to claim 1, is characterized in that, described ASA and the weight ratio of MAH are (70～80): (20～30).
7. method according to claim 1, is characterized in that, described PPR and the weight ratio of MWCNT are (70～95): (5～30).
8. method according to claim 3, is characterized in that, described oxidation inhibitor is one or more in Hinered phenols antioxidant and phosphite ester kind antioxidant; Described lubricant be fatty acid ester or oxidized polyethlene wax one or more; Described anti ultraviolet agent is one or more of benzotriazole category, triazines, benzophenone, hindered amines; Described thermo-stabilizer be organic tin thermo-stabilizer, metal soap thermal stabilizers one or more.
9. polycarbonate/the third alkene nitrile ?benzene second alkene ?acrylate graft copolymers the alloy preparing according to method described in above-mentioned arbitrary claim, it is characterized in that, the socle girder notched Izod impact strength of this alloy is greater than 650J/m under 23 ℃ of environment, and surface resistivity reaches 10
9ohm, reaches 10 through 90 ℃, 96RH% fixed temperature and humidity 24h hydrolysis reaction rear surface resistance
9ohm, there is not being hydrolyzed phenomenon in material.
10. according to an application for the polycarbonate/the third alkene nitrile ?benzene second alkene ?acrylate graft copolymers alloy described in above-mentioned arbitrary claim, it is characterized in that, use it for and prepare inner and outer decorative parts of automobile or outdoor activity sports equipment goods.
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