CN100374504C - Poycarbonate/montmorillonite nano composite materials and method for preparing same - Google Patents
Poycarbonate/montmorillonite nano composite materials and method for preparing same Download PDFInfo
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Abstract
The present invention discloses a polycarbonate / montmorillonite nanometer composite material which is mainly composed of 5 wt% to 35 wt% of grafting polyolefin-based montmorillonite master batch and 65 wt% to 95 wt% of polycarbonate resin, wherein the grafting polyolefin-based montmorillonite master batch is mainly composed of 15 wt% to 50 wt% of purified montmorillonite or organic montmorillonite containing alkyl quaternary ammonium salt, 10 wt% to 35 wt% of epoxy compound and 30 wt% to 70 wt% of grafting polyolefin. The present invention also discloses the preparation method of the composite material, which comprises: adding the organic montmorillonite or the purified montmorillonite into the epoxy compounds to be mixed to form epoxidated organic montmorillonite; adding the mixture in grafting polyalkylene-based body for melt extrusion; mixing polymer-based montmorillonite master batch with polycarbonate at 190 DEG C to 250 DEG C after the polymer-based montmorillonite master batch is prepared; forming the composite material by melt extrusion and granulation. The mechanical property of the composite material is enhanced obviously, and the chemical property, such as stress crack-resistant property, is largely improved.
Description
Technical field
The invention belongs to technical field of composite materials, specifically relate to a kind of polycarbonate/Nanometer Composite Material Of Montmorillonite And Its Preparation Method.
Background technology
Polycarbonate resin (PC) is the chain macromolecule compound that contains the carbonic ether chain link in the molecular backbone chain.At present, have practical value and the kind of suitability for industrialized production only for bisphenol A polycarbonate.The world 4 big polycarbonate resin production company is U.S. GE company, German Bayer company, U.S. DOW chemical company and Japanese Supreme Being people chemical company.
The PC resin material has many excellent properties, is a kind of engineering plastics of excellent property.Yet because the high rigidity of phenyl ring and big sterically hindered etc. influence on the PC resin macromolecular main chain, the crystallizing power of PC resin is poor, melt viscosity is very high, cause the processing rheological of PC resin poor, easy to crack, solvent resistance and wearability are relatively poor, therefore the PC study on the modification are become the most important problem of PC applied research.The property modification research of PC resin mainly is the following aspects: processing fluidity and the forming process of improving PC; Improve fatigue resistance and hardness; Improve the heavy wall pipe low-temperature impact toughness, reduce notch sensitivity; Improve solvent resistance and stress cracking resistance; Improve wear resistance, improve Young's modulus.
Modification PC kind mainly comprises enhancing PC and PC alloy two big classes, and wherein the PC alloying is the important channel of PC modification.Improving the processibility of PC, improve notch sensitivity and stress cracking resistance, reduce cost, is the major objective of PC alloying.The research of PC alloying mainly contains: (1) PC/ABS alloy.PC and ABS blend be the premium properties of PC and ABS comprehensively, reduces PC resin melt viscosity, improves processing characteristics, improves the stress cracking resistance of PC, reduces the susceptibility of impacting thickness and breach, also reduces cost simultaneously.(2) PC/PS alloy.In PC, add PS and can reduce the PC viscous flow activation energy, reduce melt viscosity, improve the processing fluidity of PC greatly, thereby improve the formability of PC.PS can also play the effect of Rigid Organic Fillers in PC, improve the hardness of PC.(3) PC/PBT, PC/PET alloy.PBT has excellent characteristics such as mechanical property, resistance to chemical attack and easy-formation, with PBT and PC blend make that alloy material can improve the PC flowability, improves processing characteristics, stress cracking resistance and chemical proofing.PET has mechanical property and chemical proofing preferably, and the rigidity of the existing PC of PC/PET and thermotolerance the solvent resistance of PET is arranged again, and the adding of PET can also be improved the processing fluidity of PC.(4) PC/PO alloy.The PC/PO alloy comprises PC/PE alloy and PC/PP alloy, and PC and PO blend can improve the shock resistance of PC, improve the processing fluidity of PC, reduce the internal stress of goods, can also improve tensile strength and the elongation at break of PC simultaneously, and reduces the cost of PC.(5) PC/PA alloy.In PC, add PA, can improve oil-proofness, chemical-resistant, stress cracking resistance and the processing characteristics of PC, reduce the cost of PC, keep the higher shock-resistant and thermotolerance of PC simultaneously.(6) PC/POM alloy.PC/POM alloy organic solvent-resistant ability significantly improves, and has improved the stress cracking resistance of polycarbonate.
Since the eighties in 20th century, each major company's emphasis of the world is researched and developed bisphenol A polycarbonate multipolymer and polycarbonate alloy, develops many modified polycarbonate kinds with special performance, remarkable in economical benefits.At present, make rapid progress, also have multiple PC alloy constantly to be developed and to introduce to the market about the research and development of PC alloy.Use glass fibre and PC is carried out enhancing modified research obtain good effect and achievement equally, the commercial products that release one after another such as U.S. GE company, German Bayer company, U.S. DOW chemical company, Japanese Supreme Being people chemical company, BASF AG, Mitsubishi Chemical Ind.
The applying nano materials modified engineered plastic as PA, PET, PBT etc., since the eighties in 20th century, has carried out this both at home and abroad studying extensively and profoundly, and has obtained a series of achievements.Wherein the successful Application of nano material in resins such as PA, PS, PO, PET, PBT, PVC prepared high performance nano composite material, allows the researchist see hope.Applying nano materials modification PC, improve notch sensitivity and stress cracking resistance to obtain, improve Young's modulus, improve the effects such as processibility of PC, become the research focus gradually, each major company, each big research institution and each big colleges and universities are all carrying out systematic research both at home and abroad.What the research report was wherein arranged is: German Bayer AG uses high-purity talc and wollastonite has been succeeded in developing modification PC resin, and the patent No. is CN1413228A " flame-resistant polycarbonate molding compositions that comprises high-purity talc ", CN1434841A " polycarbonate molding compositions that contains special talc " and CN1575317A " the impact-resistant modified polycarbonate Alloys of mineral enhanced ".The nano clay modified PC resin of Cornell Univ USA's research in nanotechnology center applications surface-treated, the thermal stability problems of solution clay, the good nano composite material of preparation rerum natura, wherein the toughness of material is higher by 30% than general PC composite material.Reported " the SiO of Zhou Chongguang of Shandong University etc. in the 16th phase of February in 2000 " macromolecular material and engineering "
2The preparation of/polycarbonate nano phase composite materials and performance ", prepared SiO by sol-gel process
2/ PC matrix material, TEM (transmission electron microscope) analysis show, SiO
2The particles dispersed that forms 300-400nm is in PC external phase.Thermogravimetic analysis (TGA) shows that the thermostability of material is with SiO
2The increase of content and improving.Torsion(al)braid analysis shows that the second-order transition temperature of material improves more than 20 ℃ than PC.
Summary of the invention
The invention provides a kind of graft polyolefin base montmorillonite masterbatch material modified as polycarbonate resin of adopting, prepare high performance polycarbonate/Nano composite material of montmorillonite.
The present invention also provides the preparation method of polycarbonate/Nano composite material of montmorillonite, promptly adopt graft polyolefin base montmorillonite masterbatch, mixed in proportion with polycarbonate material, can add other processing aids, melt extrude granulation through twin screw, preparation polycarbonate/Nano composite material of montmorillonite.
A kind of polycarbonate/Nano composite material of montmorillonite, its main raw material consists of: graft polyolefin base montmorillonite masterbatch: 5-35% (weight) polycarbonate resin: 65-95% (weight);
Consisting of of described graft polyolefin base montmorillonite masterbatch: described graft polyolefin base montmorillonite masterbatch is made up of following main materials: epoxidation organo montmorillonite 30-70% (weight), graft polyolefin: 10-35% (weight), and wherein the epoxidation organo montmorillonite is organic montmorillonoid or purification polynite and mixing cured the forming of 10-35% (weight) epoxy compounds that 15-50% (weight) is contained alkyl quaternary ammonium salts; Described organic montmorillonoid or purification polynite are the nano level polynite.
Described graft polyolefin is one or more in graft polypropylene, grafted polyethylene, grafted polystyrene and the grafted ABS.The grafting group of graft polyolefin can be a kind of in maleic anhydride, silane, vinylformic acid, polyacrylamide, maleic anhydride-styrene, the MALEIC ANHYDRIDE, and the percentage of grafting of grafting group is 0.8%-1%.
The preparation method of above-mentioned polycarbonate/Nano composite material of montmorillonite comprises:
1. the organic montmorillonoid or the purification polynite 15-50% that will contain alkyl quaternary ammonium salts mix with the weight ratio of epoxy compounds 10-35%, under 150 ℃ of-200 ℃ of temperature condition, mixing through the powerful shearing of two rollers, twin screw or Banbury mixer, be solidified into the closely knit powder-material of epoxidation organo montmorillonite;
2. epoxidation organo montmorillonite powder-material 30-70% is mixed with the weight ratio of graft polyolefin 30-70%, melt extrude and disperse to peel off formation graft polyolefin base montmorillonite masterbatch;
3. the weight ratio mixed milling that in polycarbonate 65%-95%, adds graft polyolefin base montmorillonite masterbatch 5%-35%, add other processing aids, under 190 ℃ of-250 ℃ of temperature condition, mixing through twin-screw mixer equipment, melt extrude granulation, preparation polycarbonate/Nano composite material of montmorillonite.
Described epoxidation organo montmorillonite powder-material, the inventor discloses the preparation method in patent CN03137638.X and CN200410015775.2.Use epoxy compounds as properties-correcting agent, with epoxy compounds with contain the organic montmorillonoid of alkyl quaternary ammonium salts or purification polynite and mix after, under 150 ℃ of-200 ℃ of temperature condition, mixing through the powerful shearing of two rollers, twin screw or Banbury mixer, be solidified into the closely knit powder-material of epoxidation organo montmorillonite.Its salient features has: the high temperature resistant and color-changing performance is good, can be greater than 330 degree, and polynite content is up to 50-75%, and interlamellar spacing is big, can reach 3.0-10.0nm, easily disperses to peel off in polymkeric substance.
Described graft polyolefin base montmorillonite masterbatch, be after graft polyolefin and epoxidation organo montmorillonite are mixed by a certain percentage, can add other processing aids, under 180 ℃ of-240 ℃ of temperature condition, mixing through twin-screw mixer equipment, melt extrude granulation, the graft polyolefin base montmorillonite masterbatch of preparation.
Polycarbonate resin, can adopt polycarbonate regenerated material, it also can be the polycarbonate transparent material, as the poly-transparent material of PC in the transparent material of PC, the transparent material of PC of Bayer AG, the transparent material of PC of the long wind in Chongqing, the Shen, Shanghai of GE company, Changzhou organic chemical industry's the transparent material of PC etc., require resin into general injection grade.
Polycarbonate/the Nano composite material of montmorillonite of the inventive method preparation, montmorillonite masterbatch is peeled off in polycarbonate matrix fully, and polynite is homodisperse.The mechanical property of this matrix material is significantly improved, and chemical property such as stress crack resistance performance improve significantly.
Matrix material of the present invention, through XRD (X-ray diffraction) test, 001 diffractive features peak does not appear in 2 θ angles in 1-15 °, illustrates that montmorillonite masterbatch reaches nano level substantially and disperses in polymeric matrix.
Embodiment
Embodiment 1:
Nano imvite and epoxy compounds add other processing aid in 1: 1 ratio proportioning, and be mixed mixing, preparation epoxidation organo montmorillonite.Get 50 parts of the epoxidation organo montmorillonites of preparation, 50 parts of maleic anhydride inoculated polypropylenes mixedly at a high speed join in the twin screw extruder after evenly, and extruding pelletization under 180 ℃ of-240 ℃ of temperature condition obtains graft polypropylene base montmorillonite masterbatch.
Get 12 parts of this graft polypropylene base montmorillonite masterbatch, 88 parts of polycarbonate regenerated materials, other processing aid, double-screw mixing and mixing under 190 ℃ of-250 ℃ of temperature condition melt extrudes granulation, preparation polycarbonate/Nano composite material of montmorillonite.
Embodiment 2:
Nano imvite and epoxy compounds add other processing aid in 1: 1 ratio proportioning, and be mixed mixing, preparation epoxidation organo montmorillonite.Get 60 parts of the epoxidation organo montmorillonites of preparation, 40 parts of acrylic acid-grafted polyethylene mixedly at a high speed join in the twin screw extruder after evenly, and extruding pelletization under 180 ℃ of-240 ℃ of temperature condition obtains grafted polyethylene base montmorillonite masterbatch.
Get 10 parts of this graft polypropylene base montmorillonite masterbatch, 90 parts of GE company polycarbonate, other processing aid, double-screw mixing and mixing under 190 ℃ of-250 ℃ of temperature condition melt extrudes granulation, preparation polycarbonate/Nano composite material of montmorillonite.
Embodiment 3:
Nano imvite and epoxy compounds add other processing aid in 2: 1 ratio proportionings, and be mixed mixing, preparation epoxidation organo montmorillonite.Get 50 parts of this epoxidation organo montmorillonites, 50 parts of maleic anhydride graft polystyrene, high speed joins in the twin screw extruder after mixing evenly, and extruding pelletization under 180 ℃ of-240 ℃ of temperature condition obtains grafted polystyrene base montmorillonite masterbatch.
Get 10 parts of this graft polypropylene base montmorillonite masterbatch, 90 parts of polycarbonate regenerated materials, other processing aid, double-screw mixing and mixing under 190 ℃ of-250 ℃ of temperature condition melt extrudes granulation, preparation polycarbonate/Nano composite material of montmorillonite.
Embodiment 4:
Nano imvite and epoxy compounds add other processing aid in 2: 1 ratio proportionings, and be mixed mixing, preparation epoxidation organo montmorillonite.Get 60 parts of this epoxidation organo montmorillonites, 40 parts of acrylic acid-grafted polypropylenes, high speed joins in the twin screw extruder after mixing evenly, and extruding pelletization under 180 ℃ of-240 ℃ of temperature condition obtains graft polypropylene base montmorillonite masterbatch.
Get 8 parts of this graft polypropylene base montmorillonite masterbatch, 92 parts of GE company polycarbonate, other processing aid, double-screw mixing and mixing under 190 ℃ of-250 ℃ of temperature condition melt extrudes granulation, preparation polycarbonate/Nano composite material of montmorillonite.
Embodiment 5:
Nano imvite and epoxy compounds add other processing aid in 3: 2 ratio proportionings, and be mixed mixing, preparation epoxidation organo montmorillonite.Get 50 parts of this epoxidation organo montmorillonites; 50 parts of maleic anhydride inoculated polypropylenes, high speed join in the twin screw extruder after mixing evenly, and extruding pelletization under 180 ℃ of-240 ℃ of temperature condition obtains graft polypropylene base montmorillonite masterbatch.
Get 10 parts of this graft polypropylene base montmorillonite masterbatch, 90 parts of polycarbonate regenerated materials, other processing aid, double-screw mixing and mixing under 190 ℃ of-250 ℃ of temperature condition melt extrudes granulation, preparation polycarbonate/Nano composite material of montmorillonite.
Embodiment 6:
Nano imvite and epoxy compounds add other processing aid in 3: 2 ratio proportionings, and be mixed mixing, preparation epoxidation organo montmorillonite.Get 60 parts of this epoxidation organo montmorillonites; 40 parts of maleic anhydride grafted ABS, high speed join in the twin screw extruder after mixing evenly, and extruding pelletization under 180 ℃ of-240 ℃ of temperature condition obtains grafted ABS base montmorillonite masterbatch.
Get 9 parts of this grafted ABS base montmorillonite masterbatch, 91 parts of the polycarbonate resins of GE company, other processing aid, double-screw mixing and mixing under 190 ℃ of-250 ℃ of temperature condition melt extrudes granulation, preparation polycarbonate/Nano composite material of montmorillonite.
Above-mentioned matrix material is carried out performance test:
1. with the polycarbonate/Nano composite material of montmorillonite of example 1, through XRD (X-ray diffraction) test, 001 diffractive features peak does not appear in 2 θ angles in 1-15 °, illustrates that montmorillonite masterbatch reaches nano level substantially and disperses in polymeric matrix.The Young's modulus of matrix material and tensile strength are respectively 2.0GPa and 58.0MPa, and the performance (data that provides according to GE company shows: the Young's modulus and the tensile strength of the PC241-LA888 resin of GE company are respectively 1.8-2.5GPa and 55.0-65.0Mpa) of the same level PC of GE company resin is provided.Be injection molded into product, the melt flow property improvement of polycarbonate, product is at CCl
4Soak more than 20 hours in the solution, it is tiny netted that the crackle of product is, and do not have obviously and deepen, and the PC of GE company material product obviously peeled off and come off.
2. with the polycarbonate/Nano composite material of montmorillonite of example 3, through XRD (X-ray diffraction) test, 001 diffractive features peak does not appear in 2 θ angles in 1-15 °, illustrates that montmorillonite masterbatch reaches nano level substantially and disperses in polymeric matrix.The Young's modulus of matrix material and tensile strength are respectively 2.5GPa and 60.0MPa, reach the performance of the PC241-LA888 resin of GE company.Be injection molded into product, the melt flow property improvement of polycarbonate, product is at CCl
4Soak more than 20 hours in the solution, it is tiny netted that the crackle of product is, and do not have obviously and deepen, and the PC of GE company material product obviously peeled off and come off.
3. with the polycarbonate/Nano composite material of montmorillonite of example 6, through XRD (X-ray diffraction) test, 001 diffractive features peak does not appear in 2 θ angles in 1-15 °, illustrates that montmorillonite masterbatch reaches nano level substantially and disperses in polymeric matrix.The Young's modulus of matrix material and tensile strength are respectively 3.0GPa and 63.0Mpa.Be injection molded into product, the melt flow property improvement of polycarbonate, product is at CCl
4Soak more than 20 hours in the solution, it is tiny netted that the crackle of product is, and do not have obviously and deepen, and the former PC material product of GE company obviously peeled off and come off.
Claims (3)
1. polycarbonate/Nano composite material of montmorillonite, its main raw material consists of:
Graft polyolefin base montmorillonite masterbatch: 5-35% (weight)
Polycarbonate resin: 65-95% (weight);
Consisting of of described graft polyolefin base montmorillonite masterbatch: epoxidation organo montmorillonite 30-70% (weight), graft polyolefin: 30-70% (weight), wherein the epoxidation organo montmorillonite is organic montmorillonoid or purification polynite and mixing cured the forming of 10-35% (weight) epoxy compounds that 15-50% (weight) is contained alkyl quaternary ammonium salts; Described organic montmorillonoid or purification polynite are the nano level polynite; Described graft polyolefin is one or more in graft polypropylene, grafted polyethylene, grafted polystyrene and the grafted ABS; The grafting group of described graft polyolefin is a kind of in maleic anhydride, vinylformic acid, maleic anhydride-styrene, the MALEIC ANHYDRIDE.
2. polycarbonate/Nano composite material of montmorillonite according to claim 1 is characterized in that: the percentage of grafting of the grafting group of described graft polyolefin is 0.8-1%.
3. the preparation method of polycarbonate/Nano composite material of montmorillonite according to claim 1 comprises:
(1). the organic montmorillonoid or the purification polynite 15-50% that will contain alkyl quaternary ammonium salts mix with the weight ratio of epoxy compounds 10-35%, under 150 ℃ of-200 ℃ of temperature condition, mixing through the powerful shearing of two rollers, twin screw or Banbury mixer, be solidified into the closely knit powder-material of epoxidation organo montmorillonite;
(2). 30-70% mixes with the weight ratio of graft polyolefin 30-70% with epoxidation organo montmorillonite powder-material, and fusion is sheared mixing, and polynite disperses to peel off, and extruding pelletization forms graft polyolefin base montmorillonite masterbatch;
(3). the weight ratio that adds graft polyolefin base montmorillonite masterbatch 5%-35% in polycarbonate 65%-95% is mixed, add other processing aids, under 190 ℃ of-250 ℃ of temperature condition, mixing through twin-screw mixer equipment, melt extrude granulation, preparation polycarbonate/Nano composite material of montmorillonite.
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Families Citing this family (9)
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| CN100427545C (en) * | 2006-07-27 | 2008-10-22 | 上海交通大学 | Process for preparing polycarbonate /acrylonitirle-ternary ethyl propylene rubber-styrene resin / laminated silicate nano composite material |
| CN101787192B (en) * | 2009-10-15 | 2012-05-30 | 上海锦湖日丽塑料有限公司 | Low-gloss polycarbonate styrene resin composition and preparation method thereof |
| CN101812223A (en) * | 2009-12-25 | 2010-08-25 | 上海锦湖日丽塑料有限公司 | Polycarbonate/polyethylene glycol terephthalate resin composite and preparation method |
| CN103214780B (en) * | 2013-04-25 | 2014-03-12 | 郑岩岳 | Modified ABS (acrylonitrile-butadine-styrene) special material for electric bicycle and preparation method for same |
| CN105273385A (en) * | 2015-10-26 | 2016-01-27 | 芜湖豫新世通汽车空调有限公司 | Automotive air conditioning blower casing and preparation method thereof |
| CN108660541A (en) * | 2018-06-21 | 2018-10-16 | 安徽鸿森塑业有限公司 | A kind of preparation method of low temperature resistant polypropylene woven bag |
| CN114292507B (en) * | 2021-09-27 | 2024-01-05 | 西南科技大学 | Organic montmorillonite modified flame-retardant PC material and preparation method thereof |
| CN115216044B (en) * | 2022-08-25 | 2022-12-20 | 杭州和顺科技股份有限公司 | High-light-transmission high-breakdown-voltage backboard and preparation method thereof |
| CN116444965A (en) * | 2023-04-10 | 2023-07-18 | 江苏联盟化学有限公司 | Puncture-resistant functional master batch of biodegradable plastic and preparation method and application thereof |
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Free format text: CORRECT: ADDRESS; FROM: 310013 B/F, HUAHONG BUILDING, NO.248, TIANMUSHAN ROAD, XIHU DISTRICT, HANGZHOU CITY, ZHEJIANG PROVINCE TO: 310023 NO.138, WUCHANG AVENUE, WUCHANG INDUSTRIAL PARK, YUHANG DISTRICT, HANGZHOU CITY, ZHEJIANG PROVINCE |
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Effective date of registration: 20110215 Address after: 310023 No. 138 Wuchang Road, Wuchang Industrial Zone, Yuhang District, Zhejiang, Hangzhou Co-patentee after: Hongyan Electric Appliance Co., Ltd., Hangzhou Patentee after: Zhejiang HONYAR Plastic Manufacturing Co., Ltd. Address before: 310013, B building, Huahong building, 248 Tian Tian Shan Road, Hangzhou, Zhejiang, Xihu District Patentee before: Hongyan Electric Appliance Co., Ltd., Hangzhou |
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Owner name: HONGYAN ELECTRIC APPLIANCE CO., LTD., HANGZHOU Free format text: FORMER OWNER: ZHEJIANG HONGYAN PLASTIC PRODUCING CO., LTD. Effective date: 20140703 Free format text: FORMER OWNER: HONGYAN ELECTRIC APPLIANCE CO., LTD., HANGZHOU Effective date: 20140703 |
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Free format text: CORRECT: ADDRESS; FROM: 310023 HANGZHOU, ZHEJIANG PROVINCE TO: 310013 HANGZHOU, ZHEJIANG PROVINCE |
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| TR01 | Transfer of patent right |
Effective date of registration: 20140703 Address after: 310013 B building, Huahong building, 248 Tian Tian Shan Road, Zhejiang, Hangzhou Patentee after: Hongyan Electric Appliance Co., Ltd., Hangzhou Address before: 310023 No. 138 Wuchang Road, Wuchang Industrial Zone, Yuhang District, Zhejiang, Hangzhou Patentee before: Zhejiang HONYAR Plastic Manufacturing Co., Ltd. Patentee before: Hongyan Electric Appliance Co., Ltd., Hangzhou |