CN1465618A - Magnesium hydrate halogen-free polypropylene flame redardant composite material - Google Patents
Magnesium hydrate halogen-free polypropylene flame redardant composite material Download PDFInfo
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- CN1465618A CN1465618A CNA021243921A CN02124392A CN1465618A CN 1465618 A CN1465618 A CN 1465618A CN A021243921 A CNA021243921 A CN A021243921A CN 02124392 A CN02124392 A CN 02124392A CN 1465618 A CN1465618 A CN 1465618A
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Abstract
The composition of magnesium hydroxide halogen-free fire-resisting polypropylene composite material is composed of (by weight portion) polypropylene 100, magnesium hydroxide 20-200, elastic body 5-25, coupling agent 0.1-4.0, cross-linking adjuvant 0.5-5.0, initiating agent 0.05-0.5, dispersing agent 0.5-8.0, synergist 0.2-3.0 and antioxidant 0.1-1.0. The described polypropylene is homopolymer polypropylene and copolymer polypropylene, the described magnesium hydroxide is natural ore powder or synthetic one, and its grain size is 1-100 micrometers generally, and the described elastic body is EPR, EPDM, butyl rubber ethylene-octene copolymer and ethylene-vinyl acetate copolymer, etc.
Description
Technical field the present invention relates to a kind of flame-retardant polypropylene composite material, the halogen-free flame-retardant composite material that particularly a kind of polypropylene and magnesium hydroxide are formed.
The background technology polypropylene material has proposed requirement in Application for Field such as building materials, automobile, electrical equipment to its flame retardant resistance.The general employing added the flame retardant resistance that fire retardant improves polypropylene material, used halogen system, phosphorus system, nitrogen flame retardant and the mixture thereof of mostly being, and less employing magnesium hydroxide (Mg (OH)
2), aluminium hydroxide (Al (OH)
3) halogen-free flame retardants.
People such as Gao Wenhua, Guo Xikun has reported a kind of halogen-free flame retardants magnesium hydroxide filled polypropylene material on " plastics science and technology " 1992 the 6th the 1st phases of volume, the addition of magnesium hydroxide just has flame retardant effect more than 55% (weight percentage), and increase with addition, the mechanical properties decrease of material is remarkable, magnesium hydroxide filled polypropylene material without coupling agent treatment, its tensile strength is to be lower than 10MPa at 40% o'clock at addition, after two kinds of coupling agent treatment, the tensile strength of material is also to be lower than 15MPa at 40% o'clock at addition.
United States Patent (USP) 4987173 has been reported the composite polyolefine material of fibrousness mineral filler, and its mineral filler is magnesium hydroxide, magnesium oxide, gypsum or two or more mixture, and addition can't be processed when 70% (weight percentage).
The addition of halogen-free flame retardants need reach the above just possible anti-flaming polypropylene material of 50-60% (weight percentage) in the prior art, and the above addition of 50-60% causes material mechanical performance poor, processing difficulties can not satisfy and use and the quantity-produced requirement.
Summary of the invention the objective of the invention is to overcome above-mentioned shortcoming, and a kind of magnesium hydroxide flame retardant polypropylene composite material with excellent mechanical performances and processing characteristics is provided.
Magnesium hydrate halogen-free polypropylene flame redardant composite material of the present invention, in weight part, form by following component and content thereof:
Polypropylene 100
Magnesium hydroxide 20-200
Elastomerics 5-25
Coupling agent 0.1-4.0
Crosslinking coagent 0.5-5.0
Initiator 0.05-0.5
Dispersion agent 0.5-8.0
Synergistic agent 0.2-3.0
Oxidation inhibitor 0.1-1.0
Described polypropylene is homo-polypropylene, Co-polypropylene, and its melt flow rate (MFR) is 0.2-30.0 gram/10 minutes.
Described magnesium hydroxide is natural crystal powder or synthetic magnesium hydroxide, and its granularity is generally 1 μ m-100 μ m, and best granularity is 2-10 μ m.
Described elastomerics is ethylene-propylene rubber(EPR), terpolymer EP rubber, isoprene-isobutylene rubber, styrene-butadiene rubber(SBR), paracril, chloroprene rubber, ethylene-octene copolymer, ethylene-vinyl acetate copolymer.
Described coupling agent is vinyltriethoxysilane, vinyl three [2-methoxyethoxy] silane, γ-propyl methacrylate base Trimethoxy silane, γ-amine propyl-triethoxysilicane, N-β (amine ethyl)-γ-amine propyl group-Trimethoxy silane, β-(3,4-oxygen pushing out ring hexyl)-ethyl trimethoxy silane, γ-Racemic glycidol oxygen propyl trimethoxy silicane, γ-urea propyl-triethoxysilicane, γ-mercaptopropyl trimethoxysilane.
Described crosslinking coagent is divinylbenzene, bismaleimides, diallyl phthalate, tetramethylolmethane triaryl ester, cyanuric acid tripropylene, poly-sulphonyl change nitrogen, n-formyl sarcolysine hydrochlorate repeatedly.
Described initiator is dilauroyl peroxide, benzoyl peroxide, peroxidation two uncle's butane, dicumyl peroxide, peroxide tert pivalate ester, di-isopropyl peroxydicarbonate, di-cyclohexylperoxy dicarbonate, Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile).
Described dispersion agent is hydroxy silicon oil, vinyl silicone oil, polyhutadiene, maleic anhydride graft polyhutadiene, polyolefin-wax, inclined to one side hexafluoro rubber, stearate and salt, N, one or more in the N-ethene two Unimac 5680 acid amides etc.
Described synergistic agent is one or more in metal oxides such as carbon black, graphite, talcum powder, silicate compound, zinc oxide, molybdenum oxide, ferric oxide, zinc borate, red phosphorus, the carbonate etc.
Described oxidation inhibitor is four [β-(3,5-di-tert-butyl-4-hydroxy phenyl) propionic acid] pentaerythritol ester, 1,1,3-three (2-methyl-4-hydroxyl-5-t-butyl-phenyl) butane, 4,4-thiobis (6-tertiary butyl-3-methylphenol), tetramethylolmethane diphosphite two (2,4-di-tert-butyl phenyl) compound of one or more in ester, tricresyl phosphite (2, the 4-di-tert-butyl phenyl) ester etc.
The preparation method of magnesium hydrate halogen-free polypropylene flame redardant composite material of the present invention in turn includes the following steps:
1, untreated filler places homogenizer, and will dilute good coupling agent with thinner and evenly be sprayed in proportion on the filler, high-speed stirring 10 minutes, drying, stand-by.2, polypropylene, magnesium hydroxide, elastomerics and various auxiliary agent thereof are pre-mixed in proportion, again extrude under with 200-220 ℃ processing temperature on the twin screw extruder, granulation obtains flame-retardant polypropylene composite material.
Although do not plan to be confined to theoretic explanation, the mechanism that the present invention may exist is as follows:
Surface treatment by magnesium hydroxide, the interpolation of crosslinking coagent, initiator, dispersion agent, magnesium hydroxide is dispersed in the polypropylene matrix, elastomerics is enriched in the magnesium hydroxide surface simultaneously, form elastomerics-magnesium hydroxide " soft shell-stone " structured particles, to improve the interface adhesivity between magnesium hydroxide and polypropylene, reduce a large amount of amplitudes that add the increase of polypropylene material fragility of magnesium hydroxide, thereby improve the mechanical property and the processing characteristics of magnesium hydroxide flame retardant polypropylene material.
Magnesium hydrate halogen-free polypropylene flame redardant composite material of the present invention can be used for trolley part, electric appliance casing, electrical element, building materials, upholstery.
The present invention will be further described below in conjunction with embodiment for embodiment.
Embodiment 1:
With granularity is natural mineral magnesium hydroxide powder 1200 grams of 5 μ m, and the γ-amine propyl-triethoxysilicane with 18.0 grams in homogenizer was handled 10 minutes.With magnesium hydroxide 1200 grams of handling and 600 homo-polypropylene that restrain, the ethylene-octene elastomerics of 120 grams, 19.2 the bismaleimides of gram, 1.92 the benzoyl peroxide of gram, 28.8 the maleic anhydride graft polyhutadiene of gram, 5.76 the calcium stearate of gram, 3.84 the barium stearate of gram, 5.76 the zinc oxide of gram, 3.84 the tetramethylolmethane diphosphite two (2 of gram, 4-di-tert-butyl phenyl) ester in proportion in homogenizer pre-mixing even, on twin screw extruder, extrude again, extrusion temperature is 220 ℃, water-cooled, granulation obtains flame-retardant polypropylene composite material.The mechanical property of gained material, processing characteristics and flame retardant resistance data see Table 1.
Embodiment 2:
With granularity is natural mineral magnesium hydroxide powder 1200 grams of 5 μ m, and the γ-propyl methacrylate base Trimethoxy silane with 18.0 grams in homogenizer was handled 10 minutes.With magnesium hydroxide 1200 grams of handling and the homo-polypropylene of 600 grams, the ethylene-vinyl acetate elastomerics of 120 grams, the divinylbenzene of 19.2 grams, the benzoyl peroxide of 1.92 grams, the vinyl silicone oil of 28.8 grams, the N of 3.84 grams, the tetramethylolmethane diphosphite two (2 of the zinc oxide of N-ethene two Unimac 5680 acid amides, 5.76 grams, 3.84 grams, 4-di-tert-butyl phenyl) ester in proportion in homogenizer pre-mixing even, on twin screw extruder, extrude again, extrusion temperature is 200 ℃, water-cooled, granulation obtains flame-retardant polypropylene composite material.The mechanical property of gained material, processing characteristics and flame retardant resistance data see Table 1.
Embodiment 3:
To synthesize magnesium hydroxide powder 1200 grams, the γ-Racemic glycidol oxygen propyl trimethoxy silicane with 18.0 grams in homogenizer was handled 10 minutes.With magnesium hydroxide 1200 grams of handling and the homo-polypropylene of 600 grams, the terpolymer EP rubber of 120 grams, the bismaleimides of 19.2 grams, the benzoyl peroxide of 1.92 grams, the hydroxy silicon oil of 28.8 grams, the calcium stearate of 5.76 grams, the barium stearate of 3.84 grams, the zinc oxide of 5.76 grams, the tetramethylolmethane diphosphite two (2 of 3.84 grams, 4-di-tert-butyl phenyl) ester in proportion in homogenizer pre-mixing even, on twin screw extruder, extrude again, extrusion temperature is 220 ℃, water-cooled, granulation obtains flame-retardant polypropylene composite material.The mechanical property of gained material, processing characteristics and flame retardant resistance data see Table 1.
Embodiment 4:
With granularity is natural mineral magnesium hydroxide powder 1200 grams of 5 μ m and the homo-polypropylene of 600 grams, the ethylene-octene elastomerics of 120 grams, the tetramethylolmethane diphosphite two (2 of 3.84 grams, 4-di-tert-butyl phenyl) ester in proportion in homogenizer pre-mixing even, on twin screw extruder, extrude again, extrusion temperature is 220 ℃, water-cooled, granulation obtains flame-retardant polypropylene composite material.The mechanical property of gained material, processing characteristics and flame retardant resistance data see Table 1.
The mechanical property of table 1 polymer materials, processing characteristics and flame retardant resistance data embodiment notch shock stretch to rupture by force and stretch flexural strength modulus in flexure melting index
The long rate of anti-flammability numbering intensity (J/m) degree (MPa) (%) is (MPa) (g/10min) 1 129.6 23.0 84.9 33.4 1301.9 0.2 FV-02,102.0 16.8 39.5 24.0 1118.4 0.3 FV-13,77.0 16.2 67.4 25.4 1149.1 1.6 FV-14,35.0 17.3 41.3 26.8 1468.0 0.1 FV-1 (MPa)
Claims (10)
1. magnesium hydrate halogen-free polypropylene flame redardant composite material, in weight part, form by following component and content thereof:
Polypropylene 100
Magnesium hydroxide 20-200
Elastomerics 5-25
Coupling agent 0.1-4.0
Crosslinking coagent 0.5-5.0
Initiator 0.05-0.5
Dispersion agent 0.5-8.0
Synergistic agent 0.2-3.0
Oxidation inhibitor 0.1-1.0
2. according to the matrix material of claim 1, it is characterized in that: described polypropylene is homo-polypropylene, Co-polypropylene, and its melt flow rate (MFR) is 0.2-30.0 gram/10 minutes.
3. according to the matrix material of claim 1, it is characterized in that: described magnesium hydroxide is natural crystal powder or synthetic magnesium hydroxide, and its granularity is 1 μ m-100 μ m.
4. according to the matrix material of claim 1, it is characterized in that: described elastomerics is ethylene-propylene rubber(EPR), terpolymer EP rubber, isoprene-isobutylene rubber, styrene-butadiene rubber(SBR), paracril, chloroprene rubber, ethylene-octene copolymer, ethylene-vinyl acetate copolymer.
5. according to the matrix material of claim 1, it is characterized in that: described coupling agent is vinyltriethoxysilane, vinyl three [2-methoxyethoxy] silane, γ-propyl methacrylate base Trimethoxy silane, γ-amine propyl-triethoxysilicane, N-β (amine ethyl)-γ-amine propyl group-Trimethoxy silane, β-(3,4-oxygen pushing out ring hexyl)-ethyl trimethoxy silane, γ-Racemic glycidol oxygen propyl trimethoxy silicane, γ-urea propyl-triethoxysilicane, γ-mercaptopropyl trimethoxysilane.
6. according to the matrix material of claim 1, it is characterized in that: described crosslinking coagent is divinylbenzene, bismaleimides, diallyl phthalate, tetramethylolmethane triaryl ester, cyanuric acid tripropylene, poly-sulphonyl change nitrogen, n-formyl sarcolysine hydrochlorate repeatedly.
7. according to the matrix material of claim 1, it is characterized in that: described initiator is dilauroyl peroxide, benzoyl peroxide, peroxidation two uncle's butane, dicumyl peroxide, peroxide tert pivalate ester, di-isopropyl peroxydicarbonate, di-cyclohexylperoxy dicarbonate, Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile).
8. according to the matrix material of claim 1, it is characterized in that: described dispersion agent is hydroxy silicon oil, vinyl silicone oil, polyhutadiene, maleic anhydride graft polyhutadiene, polyolefin-wax, inclined to one side hexafluoro rubber, stearate and salt, N, one or more in the N-ethene two Unimac 5680 acid amides.
9. according to the matrix material of claim 1, it is characterized in that: described synergistic agent is one or more in metal oxide, zinc borate, red phosphorus, the carbonates such as carbon black, graphite, talcum powder, silicate compound, zinc oxide, molybdenum oxide, ferric oxide.
10. according to the matrix material of claim 1, it is characterized in that: described oxidation inhibitor is four [β-(3,5-di-tert-butyl-4-hydroxy phenyl) propionic acid] pentaerythritol ester, 1,1,3-three (2-methyl-4-hydroxyl-5-t-butyl-phenyl) butane, 4, the compound of one or more in 4-thiobis (6-tertiary butyl-3-methylphenol), tetramethylolmethane diphosphite two (2,4-di-tert-butyl phenyl) ester, tricresyl phosphite (2, the 4-di-tert-butyl phenyl) ester.
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| CNB021243921A CN1189510C (en) | 2002-06-21 | 2002-06-21 | Magnesium hydrate halogen-free polypropylene flame redardant composite material |
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|---|---|---|---|
| CNB021243921A CN1189510C (en) | 2002-06-21 | 2002-06-21 | Magnesium hydrate halogen-free polypropylene flame redardant composite material |
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| CN1189510C CN1189510C (en) | 2005-02-16 |
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| CN101307219A (en) * | 2007-05-16 | 2008-11-19 | 南通江洲工程材料科技有限公司 | Multicomponent high molecular composite construction sealing materials and production process thereof |
| CN100455896C (en) * | 2004-09-21 | 2009-01-28 | 乐金电子(天津)电器有限公司 | Coffee apparatus casing for integrated coffee apparatus and microwave oven |
| CN100564439C (en) * | 2006-07-07 | 2009-12-02 | 江苏技术师范学院 | Environment-friendly type flame-retardant plastic and preparation method thereof |
| CN101845174A (en) * | 2010-05-31 | 2010-09-29 | 江苏凯诺电缆集团有限公司 | Sheath material of solar photovoltaic cable and cable |
| CN101845175A (en) * | 2010-06-08 | 2010-09-29 | 武汉工程大学 | Template of waste and old polypropylene plastics for construction and production process thereof |
| CN101210079B (en) * | 2006-12-31 | 2010-10-13 | 大连亚泰科技新材料有限公司 | Mg(OH)2 inorganic anti-flaming material and its preparing method and application |
| CN1939963B (en) * | 2005-09-30 | 2011-05-11 | Ls电线有限公司 | Flame retardant resin composition with improved whitening resistance in bending deformation |
| CN102234398A (en) * | 2011-06-20 | 2011-11-09 | 广东榕泰实业股份有限公司 | Flame-retardant polypropylene plastic composition and preparation method thereof |
| CN102234394A (en) * | 2011-04-18 | 2011-11-09 | 刘立文 | Calcium sulfate whisker modified polypropylene composite material and preparation method thereof |
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| CN102807707A (en) * | 2012-08-12 | 2012-12-05 | 深圳市沃尔核材股份有限公司 | Halogen-free flame-retarded polypropylene foam and preparation method thereof |
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| CN103160026A (en) * | 2013-04-06 | 2013-06-19 | 浙江通力改性工程塑料有限公司 | Halogen-free flame retardant polypropylene composition |
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| CN106397997A (en) * | 2016-08-31 | 2017-02-15 | 宁波国海电子有限公司 | Halogen-free thermoplastic elastomer cable material and preparation method thereof |
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| CN114672099A (en) * | 2022-02-22 | 2022-06-28 | 金发科技股份有限公司 | Magnesium hydroxide master batch and preparation method and application thereof |
-
2002
- 2002-06-21 CN CNB021243921A patent/CN1189510C/en not_active Expired - Fee Related
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| CN100455896C (en) * | 2004-09-21 | 2009-01-28 | 乐金电子(天津)电器有限公司 | Coffee apparatus casing for integrated coffee apparatus and microwave oven |
| CN1939963B (en) * | 2005-09-30 | 2011-05-11 | Ls电线有限公司 | Flame retardant resin composition with improved whitening resistance in bending deformation |
| CN100564439C (en) * | 2006-07-07 | 2009-12-02 | 江苏技术师范学院 | Environment-friendly type flame-retardant plastic and preparation method thereof |
| CN101210079B (en) * | 2006-12-31 | 2010-10-13 | 大连亚泰科技新材料有限公司 | Mg(OH)2 inorganic anti-flaming material and its preparing method and application |
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| CN102234394A (en) * | 2011-04-18 | 2011-11-09 | 刘立文 | Calcium sulfate whisker modified polypropylene composite material and preparation method thereof |
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| CN111205565B (en) * | 2020-02-21 | 2022-10-25 | 青岛竣翔新材料有限公司 | Dynamic vulcanized halogen-free flame-retardant insulator sheath, umbrella skirt composite material and preparation method |
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