CN101020774A - Environment friendly fireproof composite polypropylene material and its prepn process - Google Patents
Environment friendly fireproof composite polypropylene material and its prepn process Download PDFInfo
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Abstract
The present invention discloses one kind of green fireproof composite polypropylene material, which consists of grafting polyolefin-base montmorillonite master batch 5-10 wt%, glass fiber 5-15 wt%, no-halogen expanding fire retardant 25-35 wt%, polypropylene resin 35-64 wt% and machining assistant 1-5 wt%. The green fireproof composite polypropylene material has completely stripped montmorillonite master batch, and montmorillonite, glass fiber and fire retardant homogeneously dispersed in polypropylene base. It has fire retarding performance up to UL-94 V0 level, high mechanical performance and excellent electrical performance.
Description
Technical field
The invention belongs to technical field of composite materials, specifically relate to a kind of level polypropylene/montmorillonoid/glass fibre environmental-protection flame-retardant matrix material and preparation method thereof.
Background technology
Polypropylene is one of five big resins for universal use, have good characteristics such as light weight, easily processing, chemical proofing be strong, obtained using widely at industrial circles such as chemical industry, electrical equipment, packings, but along with the expanded demand of polypropylene in industries such as building, automobile, boats and ships and electrical apparatus insulation materials, people have higher requirement to its flame retardant properties.Itself belongs to inflammable material polypropylene, and its oxygen index is 17.0-18.0% only, and charring rate is low, produces molten drop during burning, so all will carry out flame-retardant modified to it in a lot of application scenarios.Particularly become the WEEE of the European Union instruction (2002/96/EC number instruction of European Union) of the formal law of European Union and the promulgation of ROHS instruction (2002/95/EC number instruction of European Union) from February 13rd, 2003, strict more to the requirement of polypropylene fire retardant composition.
Polyacrylic flame-retardant modified a lot of technology that have, but the most with practical value and obtained the method that heavy industrialization is used at present in these technology are to add additive flame retardant or add reactive flame retardant when polypropylene is mixed when synthetic polypropylene.At present, being used for polyacrylic fire retardant has halogenated flame retardant and halogen-free flame retardants, and wherein the applied research of halogenated flame retardant in polypropylene obtained very big success, and flame retardant effect is very desirable, and principal item has decabromodiphynly oxide, eight bromo ether, clorafin etc.But the smog that halogenated flame retardant produces in fire-retardant process is big, and poisonous, comprises carbon monoxide, aldehydes, dioxin etc., has caused " secondary harm " for people's the security of the lives and property.Along with the enhancing day by day of people's awareness of safety and environmental consciousness, halogen-free flameproof becomes a trend of the current development of polypropylene.At present the polyacrylic halogen-free flame retardants that is used for of research mainly contains following several big class: (1) inorganics fire retardant, comprise aluminium hydroxide, magnesium hydroxide etc., and wherein the Yao Jialiang of Beijing University of Chemical Technology, Qingdao University of Science and Technology etc. has certain research to this; (2) siliceous flame-retardant system, silicon-containing compound are called as " environmental friendliness " type fire retardant material, and the research of the SFG-100 of General Electric Apparatus Co.(U.S.A.), the DCRM series of U.S. DOW company, (APP/PER) intumescent system polypropylene flame redardant of Wei Ping etc. is wherein arranged; (3) halogen-free expansion fire retardant, this based flame retardant are the polypropylene fire retardant agent that is expected most and has very much future in engineering applications at present.Mainly contain ammonium polyphosphate (APP), trimeric cyanamide (MA), trihydroxyethyl isocyanuric acid ester (THEIC), Spinflam MF82, expanded polystyrene veneer graphite (EC), melamine phosphate (MPP), zinc borate etc.
The research of environment-friendly halogen-free flame-proof polypropylene composite material, mainly contain: YangTang etc. have studied melamine phosphate and the synergistic effect of nano imvite in acrylic plastering, show that its mechanism may be the structure that polynite and melamine phosphate generate aluminum phosphate and similar ceramic-like, thereby promoted the raising of carbonization amount and carbonization efficient; Li Shuhong utilizes trimeric cyanamide to make the Melamine Polyphosphate fire retardant, and with tetramethylolmethane cage shape phosphoric acid ester compositional flame-retardant polypropylene, fire-retardant rank can reach the V-0 level; Liao Rongkai etc. melt into ammonium polyphosphate modifying with ammonium polyphosphate altogether with trimeric cyanamide, add in the acrylic plastering, have made thermostability height, the low polypropylene flame redardant of moisture absorption, and flame retardant effect is good; North America Chemie Linz company has developed nitrogen-phosphorus fire retardant P-46, and when massfraction is that 25% P-46 fire retardant adds in the polypropylene, flame retardant resistance is a UL94 V-0 flame retardant grade, and mechanical property is good; The patent of Kanaoka, the Kunio etc. of Japan shows that it is fire-retardant to adopt ammonium polyphosphate flame retardant that the rare multipolymer of ethene-third is carried out, and oxygen index is reached more than 31.0; The Ou Yuxiang of Beijing Institute of Technology adopts the halogen-free expansible graphite fire retardant under red phosphorus synergist synergy, to the polyacrylic fire-retardant good flame effect that has; The nanometric magnesium hydroxide of Beijing University of Chemical Technology's development and ultra-fine red phosphorus cooperative flame retardant polypropylene material add more a spot of this flame-retardant system and can keep the original basic mechanical performance of material by the evaluation of Beijing, can well play fire retardation again; Gilman, Marosi etc. have studied the flame retardant properties of polynite/nanometer composite polypropylene material, the fire retardant mechanism of Nano composite material of montmorillonite is to condense the charcoal that coordinates, promptly when polymkeric substance is heated burning, polynite is deposited on polymer surfaces, play effect heat insulation, oxygen barrier, can obtain the polypropylene flame redardant of UL94 V-0 level.
It is to be expected most at present and to have very much future in engineering applications that halogen-free expansion fire retardant is used in the research of polypropylene material, wherein utilize the feature of layered silicate, by intercalation polymeric the nano silicone hydrochlorate is scattered in and forms matrix material in the polypropylene matrix, this polypropylene/laminated nm-silicate composite material can improve the mechanical property and the compatible performance of material, and this method has been opened up the new way of anti-flaming polypropylene material.
Summary of the invention
The invention provides a kind of employing graft polyolefin base montmorillonite masterbatch, glass fibre and halogen-free expansion fire retardant as the MODIFICATION OF POLYPROPYLENE material, preparation high-performance environmentally-friendly type flame-retardant polypropylene composite material.
The present invention also provides the preparation method of environment friendly fireproof composite polypropylene material, promptly adopt graft polyolefin base montmorillonite masterbatch, glass fibre and halogen-free expansion fire retardant, be mixed in proportion with polypropylene material, can add other processing aids, melt extrude granulation through twin screw, the preparation environment friendly fireproof composite polypropylene material.
A kind of environment friendly fireproof composite polypropylene material, weight percent consists of:
Graft polyolefin base montmorillonite masterbatch 5%-10%
Glass fibre 5%-15%
Halogen-free expansion fire retardant 25%-35%
Acrylic resin 35%-64%
Processing aid 1%-5%
Described graft polyolefin base montmorillonite master batch weight per-cent is formed:
Polynite 15-50%
Epoxy compounds 10-35%
Graft polyolefin 30-70%
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 one or more 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%.
Described glass fibre is the alkali-free long glass fibres.
Described halogen-free expansion fire retardant is nitrogen, phosphorus expanding fire retardant, and main component is ammonium polyphosphate (APP), tetramethylolmethane (PER) and trimeric cyanamide (MA).
Described processing aid comprises in oxidation inhibitor, lubricant or the compatilizer one or more.
A kind of preparation method of environment friendly fireproof composite polypropylene material 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 polymer-based carbon montmorillonite masterbatch;
3. the weight ratio mixed milling that in polypropylene 35%-64%, adds polymer-based carbon montmorillonite masterbatch 5%-10%, glass fibre 5%-15%, halogen-free expansion fire retardant 25%-35% and other processing aid 1%-5%, under 180 ℃ of-200 ℃ of temperature condition, mixing through twin-screw mixer equipment, melt extrude granulation, the preparation environment friendly fireproof composite polypropylene material.
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, the inventor discloses the preparation method in patent CN200510061489.4.After application graft polyolefin and epoxidation organo montmorillonite mix by a certain percentage, can add other processing aids, mixing through twin-screw mixer equipment under 180 ℃ of-240 ℃ of temperature condition, melt extrude granulation, the polymer-based carbon montmorillonite masterbatch of preparation.
Described acrylic resin is general injection grade, as F401, the F3045 of Zhenghai refinery, the T30S of Dushanzi, Xinjiang etc. of Shanghai petrochemical industry.
Described glass fibre is the alkali-free long glass fibres, as Mount Taishan glass, Tongxiang megalith and skies glass etc.
Described halogen-free expansion fire retardant is nitrogen, phosphorus expanding fire retardant, as medium blue research institute in morning, the Jinan rising sun in morning, Albemarle Corporation etc.
The environment friendly fireproof composite polypropylene material of the inventive method preparation, montmorillonite masterbatch is peeled off in polypropylene matrix fully, polynite, glass fibre and fire retardant homodisperse in polypropylene matrix.The flame retardant rating of this matrix material reaches UL-94 V0 level; Mechanical property is maintained and improves, and the change of taking off of certain performance does not take place; The electric property excellence.
Specific implementation method
Embodiment 1:
Polynite and epoxy compounds add other processing aid in 3: 1 ratio proportionings, 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 the graft polypropylene montmorillonite masterbatch.
Get 6 parts of this graft polypropylene montmorillonite masterbatch, 54 parts of polypropylene (F3045), 8 parts in glass fibre, 30 parts of nitrogen phosphorus fire retardants, 2 parts of other processing aids (comprising oxidation inhibitor, lubricant and compatilizer), double-screw mixing and mixing under 180 ℃ of-200 ℃ of temperature condition melt extrudes granulation, the preparation environment friendly fireproof composite polypropylene material.
Embodiment 2:
Polynite and epoxy compounds add other processing aid in 2: 1 ratio proportionings, 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 the graft polypropylene montmorillonite masterbatch.
Get 8 parts of this graft polypropylene montmorillonite masterbatch, 52 parts of polypropylene (F401), 10 parts in glass fibre, 28 parts of nitrogen phosphorus fire retardants, 2 parts of other processing aids (comprising oxidation inhibitor, lubricant and compatilizer), double-screw mixing and mixing under 180 ℃ of-200 ℃ of temperature condition melt extrudes granulation, the preparation environment friendly fireproof composite polypropylene material.
Performance test:
With the environment friendly fireproof composite polypropylene material among the embodiment 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.Matrix material is tested its flame retardant rating by the UL-94 standard method, reaches UL-94 V0 level, and oxygen index is greater than 33%; More than the tensile strength 30Mpa, more than the flexural strength 65Mpa; Heat-drawn wire reaches 160 ℃ (0.45Mpa), and vicat softening temperature reaches 150 ℃ (10N).
Claims (10)
1, a kind of environment friendly fireproof composite polypropylene material, weight percent consists of:
Graft polyolefin base montmorillonite masterbatch 5%-10%
Glass fibre 5%-15%
Halogen-free expansion fire retardant 25%-35%
Acrylic resin 35%-64%
Processing aid 1%-5%
2, environment friendly fireproof composite polypropylene material as claimed in claim 1 is characterized in that: described graft polyolefin base montmorillonite master batch weight per-cent is formed:
Polynite 15-50%
Epoxy compounds 10-35%
Graft polyolefin 30-70%
3, environment friendly fireproof composite polypropylene material as claimed in claim 2 is characterized in that: described polynite is the nano level polynite.
4, environment friendly fireproof composite polypropylene material as claimed in claim 2 is characterized in that: described graft polyolefin is one or more in graft polypropylene, grafted polyethylene, grafted polystyrene or the grafted ABS.
5, as claim 2,4 described environment friendly fireproof composite polypropylene materials, it is characterized in that: the grafting group of described graft polyolefin is one or more in maleic anhydride, silane, vinylformic acid, polyacrylamide, maleic anhydride-styrene or the MALEIC ANHYDRIDE.
6, environment friendly fireproof composite polypropylene material as claimed in claim 5 is characterized in that: the percentage of grafting of described grafting group is 0.8%-1%.
7, environment friendly fireproof composite polypropylene material as claimed in claim 1 is characterized in that: described glass fibre is the alkali-free long glass fibres.
8, environment friendly fireproof composite polypropylene material as claimed in claim 1 is characterized in that: described halogen-free expansion fire retardant is nitrogen, phosphorus expanding fire retardant.
9, environment friendly fireproof composite polypropylene material as claimed in claim 1 is characterized in that: described processing aid comprises one or more in oxidation inhibitor, lubricant or the compatilizer.
10, the preparation method of environment friendly fireproof composite polypropylene material as claimed in claim 1 comprises:
(1) organic montmorillonoid or the purification polynite 15-50% that will contain alkyl quaternary ammonium salts mixes 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 epoxidation organo montmorillonite powder-material;
(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 polymer-based carbon montmorillonite masterbatch;
(3) the weight ratio mixed milling of adding polymer-based carbon montmorillonite masterbatch 5%-10%, glass fibre 5%-15%, halogen-free expansion fire retardant 25%-35% and other processing aid 1%-5% in polypropylene 35%-64%, under 180 ℃ of-200 ℃ of temperature condition, mixing through twin-screw mixer equipment, melt extrude granulation, the preparation environment friendly fireproof composite polypropylene material.
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Cited By (14)
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| CN101693835A (en) * | 2009-08-25 | 2010-04-14 | 太仓市华鼎塑料有限公司 | Environment-friendly polypropylene composite material with high efficiency flame retardance |
| CN101928430A (en) * | 2010-10-14 | 2010-12-29 | 北京东方绿达科技发展有限责任公司 | Novel flame redundant material and preparation method thereof |
| CN101418100B (en) * | 2008-12-11 | 2011-05-18 | 上海金发科技发展有限公司 | Halogen-free flame retardant long glass fibre reinforcement polypropylene composite material and preparation method thereof |
| CN101747547B (en) * | 2008-12-04 | 2012-07-18 | 上海杰事杰新材料(集团)股份有限公司 | Non halogen flame retardant polyolefin/montmorillonite composite and preparation method thereof |
| CN101550249B (en) * | 2008-04-02 | 2012-07-18 | 上海化工研究院 | Halogen-free expandable fire retardant fiber glass reinforced polypropylene material and preparation method thereof |
| CN102604221A (en) * | 2012-03-13 | 2012-07-25 | 金发科技股份有限公司 | Halogen-free flame-retardant polypropylene composite for auto fuse holder, preparation method and application |
| CN102993564A (en) * | 2012-11-29 | 2013-03-27 | 浙江吉利汽车研究院有限公司杭州分公司 | Flame retardant material and preparation method thereof and automobile engine trim cover |
| CN103160029A (en) * | 2011-12-16 | 2013-06-19 | 合肥杰事杰新材料股份有限公司 | Halogen-free flame retardant antistatic reinforcing modified polypropylene material and preparation method thereof |
| CN103642125A (en) * | 2013-11-21 | 2014-03-19 | 浙江大学宁波理工学院 | Nano-clay and nitrogen phosphorus flame retardant synergistic flame retardant polypropylene material and preparation method thereof |
| CN103665569A (en) * | 2012-09-26 | 2014-03-26 | 黑龙江鑫达企业集团有限公司 | Long glass fiber reinforced polypropylene material and preparation method thereof |
| CN104650460A (en) * | 2015-03-13 | 2015-05-27 | 苏州能华节能环保科技有限公司 | Energy-saving environment-friendly material and preparation method thereof |
| CN104744820A (en) * | 2015-03-25 | 2015-07-01 | 上海应用技术学院 | Polypropylene layered silicate nanometer composite material and preparation method thereof |
| CN105623097A (en) * | 2016-03-02 | 2016-06-01 | 北京航天试验技术研究所 | Nanometer-material-compounded long-glass-fiber-reinforced polypropylene material and preparing method thereof |
| CN115490958A (en) * | 2022-09-27 | 2022-12-20 | 厦门稀土材料研究所 | Rare earth synergistic flame-retardant polypropylene composite material and preparation method and application thereof |
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| CN101550249B (en) * | 2008-04-02 | 2012-07-18 | 上海化工研究院 | Halogen-free expandable fire retardant fiber glass reinforced polypropylene material and preparation method thereof |
| CN101747547B (en) * | 2008-12-04 | 2012-07-18 | 上海杰事杰新材料(集团)股份有限公司 | Non halogen flame retardant polyolefin/montmorillonite composite and preparation method thereof |
| CN101418100B (en) * | 2008-12-11 | 2011-05-18 | 上海金发科技发展有限公司 | Halogen-free flame retardant long glass fibre reinforcement polypropylene composite material and preparation method thereof |
| CN101693835A (en) * | 2009-08-25 | 2010-04-14 | 太仓市华鼎塑料有限公司 | Environment-friendly polypropylene composite material with high efficiency flame retardance |
| CN101928430A (en) * | 2010-10-14 | 2010-12-29 | 北京东方绿达科技发展有限责任公司 | Novel flame redundant material and preparation method thereof |
| CN101928430B (en) * | 2010-10-14 | 2012-06-13 | 北京东方绿达科技发展有限责任公司 | Novel flame redundant material and preparation method thereof |
| CN103160029A (en) * | 2011-12-16 | 2013-06-19 | 合肥杰事杰新材料股份有限公司 | Halogen-free flame retardant antistatic reinforcing modified polypropylene material and preparation method thereof |
| CN103160029B (en) * | 2011-12-16 | 2016-02-03 | 合肥杰事杰新材料股份有限公司 | A kind of halogen-free flame-proof antistatic enhancing modified polypropylene material and preparation method thereof |
| CN102604221A (en) * | 2012-03-13 | 2012-07-25 | 金发科技股份有限公司 | Halogen-free flame-retardant polypropylene composite for auto fuse holder, preparation method and application |
| CN103665569A (en) * | 2012-09-26 | 2014-03-26 | 黑龙江鑫达企业集团有限公司 | Long glass fiber reinforced polypropylene material and preparation method thereof |
| CN102993564A (en) * | 2012-11-29 | 2013-03-27 | 浙江吉利汽车研究院有限公司杭州分公司 | Flame retardant material and preparation method thereof and automobile engine trim cover |
| CN102993564B (en) * | 2012-11-29 | 2014-10-15 | 浙江吉利汽车研究院有限公司杭州分公司 | Flame retardant material and preparation method thereof and automobile engine trim cover |
| CN103642125A (en) * | 2013-11-21 | 2014-03-19 | 浙江大学宁波理工学院 | Nano-clay and nitrogen phosphorus flame retardant synergistic flame retardant polypropylene material and preparation method thereof |
| CN103642125B (en) * | 2013-11-21 | 2016-02-10 | 浙江大学宁波理工学院 | Nano clay and nitrogen phosphorus flame retardant cooperative flame retardant polypropylene material and preparation method thereof |
| CN104650460A (en) * | 2015-03-13 | 2015-05-27 | 苏州能华节能环保科技有限公司 | Energy-saving environment-friendly material and preparation method thereof |
| CN104744820A (en) * | 2015-03-25 | 2015-07-01 | 上海应用技术学院 | Polypropylene layered silicate nanometer composite material and preparation method thereof |
| CN105623097A (en) * | 2016-03-02 | 2016-06-01 | 北京航天试验技术研究所 | Nanometer-material-compounded long-glass-fiber-reinforced polypropylene material and preparing method thereof |
| CN115490958A (en) * | 2022-09-27 | 2022-12-20 | 厦门稀土材料研究所 | Rare earth synergistic flame-retardant polypropylene composite material and preparation method and application thereof |
| CN115490958B (en) * | 2022-09-27 | 2023-08-15 | 厦门稀土材料研究所 | Rare earth synergistic flame-retardant polypropylene composite material and preparation method and application thereof |
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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 No. 248, Tianmu Mountain Road, hi tech Zone, Zhejiang, Hangzhou 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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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 |