CN103923376A - Dynamic vulcanized inflaming retarding nylon/ethylene vinyl acetate rubber thermoplastic elastomer and preparation method thereof - Google Patents
Dynamic vulcanized inflaming retarding nylon/ethylene vinyl acetate rubber thermoplastic elastomer and preparation method thereof Download PDFInfo
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- CN103923376A CN103923376A CN201410168242.1A CN201410168242A CN103923376A CN 103923376 A CN103923376 A CN 103923376A CN 201410168242 A CN201410168242 A CN 201410168242A CN 103923376 A CN103923376 A CN 103923376A
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- vinyl acetate
- ethylene vinyl
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- acetate rubber
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L31/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid; Compositions of derivatives of such polymers
- C08L31/02—Homopolymers or copolymers of esters of monocarboxylic acids
- C08L31/04—Homopolymers or copolymers of vinyl acetate
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- C—CHEMISTRY; METALLURGY
- 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
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/04—Thermoplastic elastomer
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Abstract
The invention relates to a dynamic vulcanized inflaming retarding nylon/ethylene vinyl acetate rubber thermoplastic elastomer and a preparation method thereof. The thermoplastic elastomer comprises nylon, ethylene vinyl acetate rubber (EVM), a bulking agent, a fire retardant and a crosslinking agent; an inflaming retarding nylon/ethylene vinyl acetate rubber thermoplastic elastomer is prepared through dynamic vulcanization by adopting an internal mixer, an open mill or screw extruder and adopting an ammonium polyphosphate/pentaerythritol/rare earth oxide system as a flame-retardant system. Compared with the prior art, the thermoplastic elastomer provided by the invention has the characteristic of oxygen index of maximally reaching 36.5, and can be widely applied to occasions such as vehicles, buildings and cables requiring inflaming retardance.
Description
Technical field
The invention belongs to field of polymer material preparing technology, relate to a kind of preparation method of dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body, refer more particularly to a kind of dynamic vulcanization nylon/ethane vinyl acetate rubber thermoplastic elastic body with better flame retardant properties.
Background technology
Thermoplastic elastomer refers to and shows at normal temperatures caoutchouc elasticity, macromolecular material that at high temperature can plasticizing forming.It can carry out machine-shaping with plastic apparatus, has the performance characteristics of vulcanized rubber simultaneously.Synthesis of Thermoplastic Elastomer by Dynamic Curing proposes (1962, USP3037954) the earliest by Gessler, in dynamic vulcanization process, the rubber components of disperse phase is under shearing action, limit disperses, limit sulfidization molding, therefore has technique simple, the feature that cost is low.
In recent years, dynamic vulcanization process is prepared Thermoplastic polyamide elastomer and is received increasing concern.The main terpolymer EP rubber of concentrating of research, paracril and polyamide blendedly prepare elastomer material by dynamic vulcanization, also has most application potential.In addition also have hydrogenated nitrile-butadiene rubber, ethylene-vinyl acetate rubber etc.USP5525668 discloses a kind of preparation method of novel thermoplastic elastomer.Be by the polyolefin elastomer dispersion of materials that contains functionalized EPM or EPDM in polyamide resin, the process of then elastomerics being vulcanized mutually.Elastomerics after crosslinked with trickle particle form be dispersed in polyamide resin mutually in, formed the mixture with thermoplastic characteristics.The blend obtaining can be for the preparation of elastomer material, without separately adding independent sulfidation one.Ethylene vinyl acetate rubber is the polar rubber that one has good oil resistance (being equivalent to the paracril of acrylonitrile content 26-34%), resistance to elevated temperatures (175 DEG C), anti-weather-aging property (being only second to terpolymer EP rubber).At present less about the elastomer material of polymeric amide/ethylene vinyl acetate rubber.CN102690479A discloses a kind of polymeric amide/ethylene vinyl acetate process for preparation of thermoplastic elastomer.But all these thermoplastic elastomers are all non-flame retardant types, thereby the flame retardant properties of the goods of producing is generally poor.Therefore in giving full play to the characteristic of thermoplastic elastomer, the flame retardant properties that how fundamentally to change this series products is the problem that needs solve.
Summary of the invention
Object of the present invention is exactly to provide a kind of dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body and method for making thereof with flame retardant properties, good workability in order to overcome the defect that above-mentioned prior art exists.
Object of the present invention can be achieved through the following technical solutions: a kind of dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body, it is characterized in that, and the composition of this thermoplastic elastomer raw material and parts by weight content are as follows:
Nylon 20-40 part;
Ethylene vinyl acetate rubber 10-80 part;
Linking agent 0.2-5 part;
Expanding material 0-50 part;
Flame-retardant system 10-100 part.
Described flame-retardant system is ammonium polyphosphate/tetramethylolmethane/rare-earth oxidation objects system, and the component in system and weight part content are:
100 parts of ammonium polyphosphates;
Tetramethylolmethane 0-40 part;
Rare earth oxide 0-10 part.
Described rare earth oxide is lanthanum trioxide, cerium oxide, Praseodymium trioxide, Neodymium trioxide, promethium oxide, Samarium trioxide, europium sesquioxide, gadolinium sesquioxide, terbium sesquioxide, dysprosium oxide, Holmium trioxide, Erbium trioxide, trioxide, ytterbium oxide, one or more in lutecium oxide; The preferred 2-5 weight part of content of described rare earth oxide.
Described nylon is for containing caprolactam monomer, binary or ternary nylon that hexanediamine hexanodioic acid monomer or sebacic acid decamethylene diamine form.
Described ethylene vinyl acetate rubber is that vinyl acetate content is the ethylene-vinyl acetate copolymer of 40%-80%.
Described linking agent is dicumyl peroxide, tertiary butyl cumene peroxide, two (t-butyl peroxy sec.-propyl) benzene, 2, two (the tertiary butyl peroxidation)-2 of 5-, two (the tertiary butyl peroxidation)-2 of 5-dimethyl-3-hexin and 2,5-, the one of 5-dimethylhexane.
Described expanding material is elastomeric-type chlorinatedpolyethylene, the maleated ethylene vinyl acetate copolyme that ethylene acrylic acid co polymer or maleic anhydride grafting ratio are 0.2-5%.
A kind of preparation method of dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body, it is characterized in that, the method comprises the following steps: take raw material according to parts by weight, adopt Banbury mixer, mill or screw extrusion press are processed, control temperature is 150-230 DEG C, and blend 7-15min can make dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body.
Described linking agent for add separately or rubber combined with ethylene vinyl acetate in advance after together with add.
Described flame-retardant system for add separately or rubber combined with ethylene vinyl acetate in advance after together with add.
Described flame-retardant system for add separately or rubber combined with ethylene vinyl acetate in advance after together with add.
The main performance index of dynamic vulcanization nylon/ethane-vinyl acetate rubber thermoplastic elastic body of the present invention is as follows:
Limiting oxygen index(LOI): 18%-40%
Tensile strength: 1-8MPa
Elongation at break: 50-200%
Compared with prior art, body material of the present invention and the fire retardant of selecting are all Halogens, therefore in material combustion process, can not produce toxic gas, and it is fire-retardant that the rare earth oxide that the present invention adopts carries out synergistic, both reduce the proportion of fire retardant in matrix, improved again the flame retardant properties of material.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
Material used: nylon 1010, the trade mark 09 type, Shanghai xylonite factory, end amido content is 34.7mol/10
6g, intrinsic viscosity be 83.4mL/g (25 DEG C, 96%H
2sO
4), relative crystallinity is 26%; Ethylene-vinyl acetate rubber (EVM400), VA content 60wt%, mooney viscosity
trade names
600, German Lanxess Corporation.Ethylene vinyl acetate copolymer grafted maleic anhydride (EVA-g-MA): vinyl acetate content 14%, maleic anhydride grafting ratio 0.72%, self-control.Ammonium polyphosphate (APP), Shanghai Xu Sen company produces, trade mark AP422, phosphorus content is 31.5%; Tetramethylolmethane (PER), traditional Chinese medicines group produces.Lanthanum trioxide (La
2o
3), Samarium trioxide (Sm
2o
3), Conghua of Guangdong Province city Jian Feng rare earth company limited produces.
Implementation step:
The first step: nylon 1010 and EVM are placed in respectively to 80 DEG C and 60 DEG C of vacuum oven 12h to remove moisture.By APP, PER, rare earth oxide after vacuum-drying dehydration, grinds 10min and mixes for subsequent use at 120 DEG C in mortar.Slice after EVM rubber is mixed in two roller mills with vulcanizing agent DCP.Then each material is taken to Nylon, EVM, EVA-g-MA, DCP, APP, PER, La according to formula in table 1
2o
3, Sm
2o
3each 30,70,15,0.8,30,10,0,0 part.
By nylon and EVA-g-MA, APP, PER, rare earth oxide is melt blending 2min in Banbury mixer, then adds a certain amount of EVM rubber unvulcanizate to carry out dynamic vulcanization 8min, 210 DEG C of temperature, rotating speed 60rpm.After mixing and finishing, material is taken off, on vulcanizing press 230 DEG C, under pressure 10MPa, be pressed into 120 × 100 × 3mm
3with 100 × 100 × 1mm
3model is for preparation combustionproperty and Mechanics Performance Testing batten.
Embodiment 2-10 is identical with two implementation steps of above-described embodiment 1 with the implementation step of comparative example 1-2, wherein Nylon, EVM, EVA-g-MA, DCP, APP, PER, La
2o
3, Sm
2o
3add according to the proportioning shown in table 1.
Table 1 has embodiment and the comparative example formula of the nylon/ethane vinyl acetate rubber thermoplastic elastic body of flame-retarding characteristic
The performance of flame retardant type thermoplastic elastomer prepared by embodiment 1-10 and comparative example 1-2 is tested according to following standard.The testing standard that embodiment 1 is adopted:
Limiting oxygen index(LOI): ASTM D2863.
Tensile strength, elongation at break: ASTM412-2006.
The performance test results of embodiment 1-10 and comparative example 1-2 is as table 2
The performance test results of table 2 embodiment 1-10 and comparative example 1-2
Embodiment 11
A preparation method for dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body, comprises the following steps:
(1) preparation of flame-retardant system: by 100 parts of ammonium polyphosphates; 1 part of tetramethylolmethane; It is for subsequent use that 1 part of rare earth oxide lutecium oxide is mixed into flame-retardant system;
(2) preparation of thermoplastic elastomer
Take 20 parts of nylon according to parts by weight; 80 parts of ethylene vinyl acetate rubber; 5 parts of linking agents; 50 parts of expanding materials; 10 parts of flame-retardant systems, adopt Banbury mixer, and control temperature is 150-160 DEG C, and blend 14-15min can make dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body.
Embodiment 12
A preparation method for dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body, comprises the following steps:
(1) preparation of flame-retardant system: by 100 parts of ammonium polyphosphates; 40 parts of tetramethylolmethanes; It is for subsequent use that 10 parts of rare earth oxide gadolinium sesquioxides are mixed into flame-retardant system;
(2) preparation of thermoplastic elastomer
Take 40 parts of nylon according to parts by weight; 10 parts of ethylene vinyl acetate rubber; 0.2 part of linking agent; 0 part of expanding material; 100 parts of flame-retardant systems, adopt mill to process, and control temperature is 220-230 DEG C, and blend 7-8min can make dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body.
Embodiment 13
A preparation method for dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body, comprises the following steps:
(1) preparation of flame-retardant system: by 100 parts of ammonium polyphosphates; 5 parts of tetramethylolmethanes; It is for subsequent use that 5 parts of rare earth oxide dysprosium oxides are mixed into flame-retardant system;
(2) preparation of thermoplastic elastomer
Take 25 parts of nylon according to parts by weight; 75 parts of ethylene vinyl acetate rubber; 1 part of linking agent; 10 parts of expanding materials; 20 parts of flame-retardant systems, adopt screw extrusion press to process, and control temperature is 150-230 DEG C, and blend 7-15min can make dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body.
Above-described embodiment is only explanation technical conceive of the present invention and feature; its object is to make the stakeholder who is familiar with this technology can understand content of the present invention and be implemented; can not limit the scope of the invention with this; the equivalence that all spirit according to the present invention are done changes and modifies, within all should being encompassed in protection scope of the present invention.
Claims (10)
1. dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body, is characterized in that, the composition of this thermoplastic elastomer raw material and parts by weight content are as follows:
Nylon 20-40 part;
Ethylene vinyl acetate rubber 10-80 part;
Linking agent 0.2-5 part;
Expanding material 0-50 part;
Flame-retardant system 10-100 part.
2. a kind of dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body according to claim 1, it is characterized in that, described flame-retardant system is ammonium polyphosphate/tetramethylolmethane/rare-earth oxidation objects system, and the component in system and weight part content are:
100 parts of ammonium polyphosphates;
Tetramethylolmethane 0-40 part;
Rare earth oxide 0-10 part.
3. a kind of dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body according to claim 2, is characterized in that, described rare earth oxide is lanthanum trioxide, cerium oxide, Praseodymium trioxide, Neodymium trioxide, promethium oxide, Samarium trioxide, europium sesquioxide, gadolinium sesquioxide, terbium sesquioxide, dysprosium oxide, Holmium trioxide, Erbium trioxide, trioxide, ytterbium oxide, one or more in lutecium oxide; The preferred 0-5 weight part of content of described rare earth oxide.
4. a kind of dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body according to claim 1, it is characterized in that, described nylon is for containing caprolactam monomer, binary or ternary nylon that hexanediamine hexanodioic acid monomer or sebacic acid decamethylene diamine form.
5. a kind of dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body according to claim 1, is characterized in that, described ethylene vinyl acetate rubber is that vinyl acetate content is the ethylene-vinyl acetate copolymer of 40%-80%.
6. a kind of dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body according to claim 1, it is characterized in that, described linking agent is dicumyl peroxide, tertiary butyl cumene peroxide, two (t-butyl peroxy sec.-propyl) benzene, 2, two (the tertiary butyl peroxidation)-2 of 5-, two (the tertiary butyl peroxidation)-2 of 5-dimethyl-3-hexin and 2,5-, the one of 5-dimethylhexane.
7. a kind of dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body according to claim 1, it is characterized in that, described expanding material is elastomeric-type chlorinatedpolyethylene, the maleated ethylene vinyl acetate copolyme that ethylene acrylic acid co polymer or maleic anhydride grafting ratio are 0.2-5%.
8. the preparation method of dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body as claimed in claim 1, it is characterized in that, the method comprises the following steps: take raw material according to parts by weight, adopt Banbury mixer, mill or screw extrusion press are processed, control temperature is 150-230 DEG C, and blend 7-15min can make dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body.
9. the preparation method of a kind of dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body according to claim 1, is characterized in that, described linking agent for add separately or rubber combined with ethylene vinyl acetate in advance after together with add.
10. the preparation method of a kind of dynamic vulcanization fire-retardant nylon/ethylene vinyl acetate rubber thermoplastic elastic body according to claim 1, it is characterized in that, described flame-retardant system for add separately or rubber combined with ethylene vinyl acetate in advance after together with add.
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Cited By (8)
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|---|---|---|---|---|
| CN104387648A (en) * | 2014-11-11 | 2015-03-04 | 合肥皖为电气设备工程有限责任公司 | Flame-retardant dielectric substrate material for printed circuit |
| CN105985568A (en) * | 2015-03-02 | 2016-10-05 | 镇江市华银仪表电器有限公司 | Anti-aging and anti-ultraviolet cable material |
| CN106220922A (en) * | 2016-08-26 | 2016-12-14 | 江苏金发科技新材料有限公司 | Dynamic vulcanization polypropylene flame redardant/nitrile rubber thermoplastic elastomer and preparation method thereof |
| CN109273160A (en) * | 2018-09-26 | 2019-01-25 | 安徽华电线缆股份有限公司 | Low temperature resistant resistance to torsion cable for wind power generation of one kind and preparation method thereof |
| CN109337185A (en) * | 2018-09-14 | 2019-02-15 | 河南科技大学 | A method of preparing halogen-free flameproof EVA/PA6 polymer alloy |
| CN109370024A (en) * | 2018-09-14 | 2019-02-22 | 河南科技大学 | A kind of toughened halogen-free flame-retardant EVA/PA6 composite material and preparation method |
| CN109370025A (en) * | 2018-09-14 | 2019-02-22 | 河南科技大学 | A kind of EVA/PA6 the flame retardant composite material and preparation method of distribution regulation improvement |
| CN112079967A (en) * | 2020-09-02 | 2020-12-15 | 池州九威新材料有限公司 | Irradiation crosslinked nylon material and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104387648A (en) * | 2014-11-11 | 2015-03-04 | 合肥皖为电气设备工程有限责任公司 | Flame-retardant dielectric substrate material for printed circuit |
| CN105985568A (en) * | 2015-03-02 | 2016-10-05 | 镇江市华银仪表电器有限公司 | Anti-aging and anti-ultraviolet cable material |
| CN106220922A (en) * | 2016-08-26 | 2016-12-14 | 江苏金发科技新材料有限公司 | Dynamic vulcanization polypropylene flame redardant/nitrile rubber thermoplastic elastomer and preparation method thereof |
| CN109337185A (en) * | 2018-09-14 | 2019-02-15 | 河南科技大学 | A method of preparing halogen-free flameproof EVA/PA6 polymer alloy |
| CN109370024A (en) * | 2018-09-14 | 2019-02-22 | 河南科技大学 | A kind of toughened halogen-free flame-retardant EVA/PA6 composite material and preparation method |
| CN109370025A (en) * | 2018-09-14 | 2019-02-22 | 河南科技大学 | A kind of EVA/PA6 the flame retardant composite material and preparation method of distribution regulation improvement |
| CN109273160A (en) * | 2018-09-26 | 2019-01-25 | 安徽华电线缆股份有限公司 | Low temperature resistant resistance to torsion cable for wind power generation of one kind and preparation method thereof |
| CN112079967A (en) * | 2020-09-02 | 2020-12-15 | 池州九威新材料有限公司 | Irradiation crosslinked nylon material and preparation method thereof |
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