CN106967230B - A kind of expanding halide-free fire-retardant, Halogen Free Flame Retardant EPDM composition and Halogen Free Flame Retardant EPDM and its application - Google Patents
A kind of expanding halide-free fire-retardant, Halogen Free Flame Retardant EPDM composition and Halogen Free Flame Retardant EPDM and its application Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5313—Phosphinic compounds, e.g. R2=P(:O)OR'
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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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Abstract
The present invention relates to flame retardant areas, specifically, it is related to a kind of expanding halide-free fire-retardant, a kind of Halogen Free Flame Retardant EPDM composition containing the expanding halide-free fire-retardant, and is kneaded by the halogen less fire retardant trielement ethylene-propylene composition and is vulcanized obtained Halogen Free Flame Retardant EPDM rubber and its application.The expanding halide-free fire-retardant contains the melamine cyanurate being mutually mixed and aluminum diethylphosphinate and/or aluminium hydroxide.Expanding halide-free fire-retardant of the invention has preferable flame retardant property, and Halogen Free Flame Retardant EPDM obtained elongation at break with higher.
Description
Technical field
The present invention relates to flame retardant areas, and in particular, to a kind of expanding halide-free fire-retardant a kind of contains the intumescent
The Halogen Free Flame Retardant EPDM composition of halogen-free flame retardants, and by halogen less fire retardant trielement ethylene-propylene composition mixing and sulphur
Change obtained Halogen Free Flame Retardant EPDM rubber and its application.
Background technique
Ethylene propylene diene rubber (EPDM) is ethylene-propylene-non-conjugated diene copolymer, has good weatherability, electricity absolutely
The performances such as edge, ozone resistance and chemical-resistant resistance, and the flame-retardant modified inflammability for being intended to overcome EPDM of EPDM improve it and answer
Safety.The fire-retardant EPDM material being commercialized at present mainly uses the flame-retardant system of bromo- antimony oxide, but halogen containing flame-retardant by
Poisonous and hazardous corrosive gas can be generated in combustion process, is just gradually abandoned by new environmental regulation, therefore recent Halogen
The research of fire-retardant EPDM is widely noticed.
Halogen-free flameproof EPDM material mostly uses greatly the magnesium hydroxide for adding environment-friendly type, aluminium hydroxide or with other cooperation at present
Agent collaboration uses.Since hydroxide flame retarding efficiency is low, relative to the EPDM of 100 parts by weight, magnesium hydroxide loading is up to 200
Parts by weight just can make EPDM reach FV-0 fire-retardant rank, at this point, the physical property of EPDM especially elongation at break becomes very poor.
Document (fine jade etc., the performance study of nano-sized magnesium hydroxide rubber composite material；Rubber industry, volume 2004,51: page 14~19)
Nano-sized magnesium hydroxide filling EPDM is reported, oxygen index (OI) can reach 30%, but elongation at break when additive amount is 150 parts by weight
Also there was only 164%.To reduce fire retardant additive amount, its flame retarding efficiency is improved, has research to add a small amount of zinc borate and makees synergist, such as
10 part by weight of boric acid zinc are added in 130 parts by weight magnesium hydroxides, and 25 part by weight of boric acid zinc are added in 105 parts by weight aluminium hydroxides,
Fire-retardant EPDM is all up FV-0, but fire retardant total amount of adding is still larger at this time；A small amount of red phosphorus, which is added, can obviously reduce hydrogen-oxygen
Compound additive amount, but the color of red phosphorus limits the use scope of product.Patent CN101928431A discloses a kind of Halogen resistance
Fire ethylene propylene diene monomer (EPDM) material, the material by expanding halide-free fire-retardant, EPDM/montmorillonite nanocomposites and
Partial phosphate ester is mixed, wherein the expanding halide-free fire-retardant, which is selected from three sources based on polyphosphoric acid amine, matches expander
System is either selected from the macromolecular structure system for integrating acid source, carbon source and gas source；The Halogen Free Flame Retardant EPDM material
Material has good anti-flammability, can reach FV-0 grades of levels, but its elongation at break also only has 200% or so.
Summary of the invention
The purpose of the present invention is overcoming, the halogen-free flame retardants dosage of the prior art is too big, flame retardant property is not good enough and/or system
At the lower problem of rubber elongation at break, a kind of expanding halide-free fire-retardant is provided, a kind of is hindered containing the expansion type halogen-free
The Halogen Free Flame Retardant EPDM composition of agent is fired, and is obtained by halogen less fire retardant trielement ethylene-propylene composition mixing and vulcanization
Halogen Free Flame Retardant EPDM rubber and its application.Expanding halide-free fire-retardant of the invention has preferable anti-flammability
Can, and Halogen Free Flame Retardant EPDM obtained elongation at break with higher.
The present invention provides a kind of expanding halide-free fire-retardant, which contains the trimerization being mutually mixed
Cyanamide cyanurate and aluminum diethylphosphinate and/or aluminium hydroxide.
The present invention also provides a kind of Halogen Free Flame Retardant EPDM composition, the Halogen Free Flame Retardant EPDM groups
It closes object and contains ethylene propylene diene rubber raw rubber and expanding halide-free fire-retardant above-mentioned.
Invention additionally provides a kind of Halogen Free Flame Retardant EPDMs, and the Halogen Free Flame Retardant EPDM is by this hair
Bright Halogen Free Flame Retardant EPDM composition is obtained by mixing and vulcanization.
The present invention also provides the application of Halogen Free Flame Retardant EPDM of the invention in electric wire, cable and automobile.
In order to improve flame retardant property and elongation at break simultaneously, the present inventor has done a large amount of exploration and has ground
Study carefully, and has been surprisingly found that during test by by melamine cyanurate and aluminum diethylphosphinate and/or hydroxide
The mating reaction of aluminium can realize good flame retardant effect, and be added the mixture as fire retardant in rubber preparation process
Obtained rubber still has good mechanical performance especially elongation at break.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The present invention provides a kind of expanding halide-free fire-retardant, which contains the trimerization being mutually mixed
Cyanamide cyanurate and aluminum diethylphosphinate and/or aluminium hydroxide.
In the present invention, the expanding halide-free fire-retardant is a kind of composition, by the way that each component to be simply mixed to obtain.
It was found by the inventors of the present invention that can by melamine cyanurate and aluminum diethylphosphinate and/or aluminium hydroxide mutual cooperation
To realize good flame retardant property, wherein the melamine cyanurate (MCA) primarily serves the effect of main flame retardant, diethyl
Base phosphinic acids aluminium (ADP) and/or aluminium hydroxide primarily serve the effect of synergist.There is no particular limitation for the content of each component,
The difference of 2 and the above order of magnitude should usually be not present between each other.For example, relative to the halogen-free intumescent flame-retardant
The content of the total weight of agent, the melamine cyanurate can be 20-90 weight %, and the aluminum diethylphosphinate contains
Amount is 0-40 weight %, and the content of the aluminium hydroxide is 0-50 weight %, and the aluminum diethylphosphinate and the hydrogen
The content of aluminium oxide is not 0 simultaneously.In the present invention, one in aluminum diethylphosphinate (ADP) and aluminium hydroxide can be selected
Kind is used cooperatively as synergist with melamine cyanurate；In situations where it is preferred, by aluminum diethylphosphinate (ADP) and
Aluminium hydroxide is used cooperatively collectively as synergist and melamine cyanurate, that is to say, that the halogen-free intumescent flame-retardant
Agent contains the melamine cyanurate being mutually mixed, aluminum diethylphosphinate and aluminium hydroxide.In this preferred situation,
Relative to the total weight of the expanding halide-free fire-retardant, the content of the melamine cyanurate can be 30-70 weight
% is measured, the content of the aluminum diethylphosphinate can be 5-40 weight %, and the content of the aluminium hydroxide can be 20-50 weight
Measure %；It is further preferred that the content of the melamine cyanurate is 40-60 weight %, the aluminum diethylphosphinate
Content be 10-20 weight %, the content of the aluminium hydroxide is 20-40 weight %.
The present invention also provides a kind of Halogen Free Flame Retardant EPDM composition, the Halogen Free Flame Retardant EPDM groups
It closes object and contains ethylene propylene diene rubber raw rubber and above-mentioned expanding halide-free fire-retardant of the invention.
In the present invention, under the premise of realizing equal or better flame retardant property and mechanical performance, the intumescent without
The content of halogen fire retardant can be substantially less than customary amount of this field using fire retardant when.In order to realize better flame resistance
And mechanical performance, in situations where it is preferred, in terms of being 100 parts by weight by the content of ethylene propylene diene rubber, expansion type halogen-free resistance
The content for firing agent is 60-160 parts by weight, more preferably 100-120 parts by weight.
In the present invention, the ethylene propylene diene rubber raw rubber can be the ethylene propylene diene rubber raw rubber of usual definition, such as
By ethylene, propylene and to can provide the copolymer that the Third monomer containing unsaturated double-bond of crosslinking sites is copolymerized, wherein institute
Stating Third monomer is, for example, ethylidene norbornene, dicyclopentadiene, 1,4- hexadiene, 3,7- dimethyl -1,6- octadiene, 5,7-
Dimethyl -1,6- octadiene or 7- methyl-1,6- octadiene etc..Wherein, ethylene propylene diene rubber life is obtained relative to for being copolymerized
Total dosage of the ethylene of glue, propylene and Third monomer, the dosage of the ethylene can be 45-80 weight %, the use of the propylene
Amount can be 15-45 weight %, and the dosage of the Third monomer can be 1-10 weight %；Preferably, relative to for being copolymerized
The ethylene of ethylene propylene diene rubber raw rubber, total dosage of propylene and Third monomer are obtained, the dosage of the ethylene can be 55-70 weight
% is measured, the dosage of the propylene can be 25-40 weight %, and the dosage of the Third monomer can be 1-5 weight %.Described three
Also there is no particular limitation for the Mooney viscosity of first EP rubbers raw rubber, such as can be 20-100, preferably 25-90.It is described " raw
Glue " continues to use the definition of this field routine, refers to rubber not through over cure, the statement for ternary resulting after vulcanization
EP rubbers distinguishes.
In the present invention, the Halogen Free Flame Retardant EPDM composition can also prepare rubber routine containing this field
The various additives of addition, the dosage of these additives is also according to the dosage of this field routine.
For example, in the present invention, the Halogen Free Flame Retardant EPDM composition can also be containing zinc oxide and/or hard
Resin acid, it is preferable that in terms of being 100 parts by weight by the content of ethylene propylene diene rubber raw rubber, the content of the zinc oxide is 3-7 weight
Part, the stearic content is 0.5-2 parts by weight.
For example, in the present invention, the Halogen Free Flame Retardant EPDM composition can also contain vulcanizing agent and/or sulphur
Change promotor, it is preferable that in terms of being 100 parts by weight by the content of ethylene propylene diene rubber raw rubber, the content of the vulcanizing agent is 0.5-2
Parts by weight, the content of the vulcanization accelerator are 0.5-3 parts by weight.The type of the vulcanizing agent is the vulcanizing agent of this field routine
Type, such as one of sulphur, peroxide and resin curative systems or a variety of can be selected from.The vulcanizing agent promotes
The type of agent be this field routine vulcanizing agent promotor type, such as can be selected from diphenyl disulfide a pair of horses going side by side thiazole (DM),
One of N- cyclohexyl -2-[4-morpholinodithio sulfenamide (CZ), thiocarbamyl sulfenamide, sulphur phosphinylidyne promotor are more
Kind；The mixture that preferably DM is mixed with CZ with 1:2-4.
Invention additionally provides a kind of Halogen Free Flame Retardant EPDMs, and the Halogen Free Flame Retardant EPDM is by this hair
Bright above-mentioned Halogen Free Flame Retardant EPDM composition is obtained by mixing and vulcanization.
In the present invention, it is described mixing and vulcanization method there is no particular limitation, according to this field routine mixing with
The method of vulcanization carries out.For example, a kind of specifically embodiment according to the present invention, the method packet of the mixing and vulcanization
Include: the ethylene propylene diene rubber raw rubber is thin 3-5 times logical on a mill, and after packet roller, adjustment roll spacing is 0.5-1.5mm, successively
Stearic acid, zinc oxide, melamine cyanurate, aluminum diethylphosphinate and aluminium hydroxide is added, is kneaded 10-12min, is added
Vulcanizing agent, promotor are kneaded uniformly, beat triangle bag 4-6 times, slice after clot 2-4 times, with flat under the conditions of 160 DEG C × 10min
The vulcanization of plate vulcanizer, can be obtained a kind of Halogen Free Flame Retardant EPDM product.
The Halogen Free Flame Retardant EPDM provided by the invention, due to the addition of expanding halide-free fire-retardant, greatly
The flame retardant property for improving material, the additive amount of fire retardant is effectively reduced, while there is good processing performance and mechanicalness
Can, to widen the application range of flame retardant ethylene propylene diene monomer (EPDM) material significantly, electric wire, cable, automobile can be widely used in
Etc. all various aspects for requiring halogen-free flameproof.
It below will the present invention is further described in detail by specific embodiment.
Embodiment 1-6 and comparative example 1-3
Dosage shown in method and table 1 is prepared as follows respectively and prepares halogen-free flameproof ternary by embodiment 1-6 and comparative example 1-3
EP rubbers product, and in addition setting is added without the blank example of fire retardant.Wherein the preparation method is that:
Take 100 parts by weight ethylene propylene diene rubber raw rubber (trade mark P750NR, Mitsui chemical products, Third monomers
Thin 4 times logical on a mill for ENB), after packet roller, adjustment roll spacing is 1mm, sequentially adds stearic acid, zinc oxide, melamine
Cyanurate (MCA), aluminum diethylphosphinate (ADP) and aluminium hydroxide are kneaded 12min, and sulphur and vulcanization accelerator (packet is added
Include DM, CZ, technical grade, Guangzhou east reddening factory products), it is kneaded uniformly, beats triangle bag 5 times, slice after clot 3 times, 160
DEG C × 10min under the conditions of vulcanized with vulcanizing press, a kind of Halogen Free Flame Retardant EPDM product can be obtained.
Table 1
Test case 1-6 and contrast test example 1-3
Test case 1-6 and contrast test example 1-3 is respectively by halogen-free flameproof three obtained by embodiment 1-6 and comparative example 1-3
First EP rubbers is tested as follows, and test result is as shown in table 2.
(1) vertical combustion time and fire-retardant rank
According to 2408-1996 test method of GB/T test vertical combustion time (s) and according to measured vertical combustion
Time (s) determines fire-retardant rank, sample size 125mm × 12.5mm × 1.6mm.
(2) oxygen index (OI) %
It is tested according to GB/T 2406-1993, sample size 85mm × 10mm × 3.2mm.
(3) shore a hardness
It is tested according to GB/T 531-1992.
(4) elongation at break and tearing strength
It is tested according to GB/T 528-1998, rate of extension 500mm/min.
Table 2
In conjunction with Tables 1 and 2 as can be seen that embodiment uses halogen-free flame retardants of the invention, by by MCA and ADP and/or
Aluminium hydroxide, which cooperates, can achieve FV-0 grades of horizontal flame retardant properties, and still has preferable elongation at break, tears
Resistance to spalling and shore a hardness；And comparative example cannot realize preferable anti-flammability when only using the one-component in fire retardant simultaneously
Energy and mechanical performance.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.It is further to note that described in above-mentioned specific embodiment
Each particular technique feature can be combined in any appropriate way in the case of no contradiction, in order to avoid not
Necessary repetition, the invention will not be further described in various possible combinations.In addition, a variety of different implementations of the invention
Any combination can also be carried out between mode, as long as it does not violate the idea of the present invention, it is public equally to should be considered as institute of the invention
The content opened.
Claims (9)
1. a kind of Halogen Free Flame Retardant EPDM composition, which is characterized in that the Halogen Free Flame Retardant EPDM composition
Containing ethylene propylene diene rubber raw rubber and expanding halide-free fire-retardant, the expanding halide-free fire-retardant contains the trimerization being mutually mixed
Cyanamide cyanurate, aluminum diethylphosphinate and aluminium hydroxide, wherein the gross weight relative to the expanding halide-free fire-retardant
Amount, the content of the melamine cyanurate are 40-60 weight %, and the content of the aluminum diethylphosphinate is 10-20 weight
% is measured, the content of the aluminium hydroxide is 20-40 weight %；
The ethylene propylene diene rubber raw rubber is by ethylene, propylene and can provide the Third monomers containing unsaturated double-bond of crosslinking sites and is total to
It is poly- to obtain, relative to total dosage for being copolymerized the ethylene for obtaining ethylene propylene diene rubber raw rubber, propylene and Third monomer, the second
The dosage of alkene is 45-80 weight %, and the dosage of the propylene is 15-45 weight %, and the dosage of the Third monomer is 1-10 weight
Measure %；The Mooney viscosity of the ethylene propylene diene rubber raw rubber is 20-100.
2. Halogen Free Flame Retardant EPDM composition according to claim 1, wherein with ethylene propylene diene rubber raw rubber
Content is 100 parts by weight meters, and the content of the expanding halide-free fire-retardant is 60-160 parts by weight.
3. Halogen Free Flame Retardant EPDM composition according to claim 2, wherein with ethylene propylene diene rubber raw rubber
Content is 100 parts by weight meters, and the content of the expanding halide-free fire-retardant is 100-120 parts by weight.
4. Halogen Free Flame Retardant EPDM composition according to claim 1 or 2, wherein the halogen-free flameproof ternary
EP rubbers composition also contains zinc oxide and/or stearic acid.
5. Halogen Free Flame Retardant EPDM composition according to claim 4, wherein with ethylene propylene diene rubber raw rubber
Content is 100 parts by weight meters, and the content of the zinc oxide is 3-7 parts by weight, and the stearic content is 0.5-2 parts by weight.
6. Halogen Free Flame Retardant EPDM composition according to claim 1 or 2, wherein the halogen-free flameproof ternary
EP rubbers composition also contains vulcanizing agent and/or vulcanization accelerator.
7. Halogen Free Flame Retardant EPDM composition according to claim 6, wherein with ethylene propylene diene rubber raw rubber
Content is 100 parts by weight meters, and the content of the vulcanizing agent is 0.5-2 parts by weight, and the content of the vulcanization accelerator is 0.5-3 weight
Measure part.
8. a kind of Halogen Free Flame Retardant EPDM, which is characterized in that the Halogen Free Flame Retardant EPDM is by claim 1-7
Any one of described in Halogen Free Flame Retardant EPDM composition by be kneaded and vulcanization obtain.
9. application of the Halogen Free Flame Retardant EPDM according to any one of claims 8 in electric wire, cable and automobile.
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| CN112592540B (en) * | 2020-12-15 | 2022-04-22 | 浙江奋飞橡塑制品有限公司 | Flame-retardant rubber for coal mine and preparation method and application thereof |
| CN114539618B (en) * | 2022-02-15 | 2023-07-11 | 东莞市宏泰基阻燃材料有限公司 | Silicone rubber halogen-free flame retardant, and preparation method and application thereof |
| CN115505215A (en) * | 2022-10-28 | 2022-12-23 | 江西奋发科技有限公司 | Low-smoke halogen-free flame-retardant rubber strip and preparation method thereof |
| CN116874878A (en) * | 2023-07-20 | 2023-10-13 | 烟台艾弗尔阻燃科技有限公司 | Flame retardant for ethylene propylene diene monomer and preparation method thereof |
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|---|---|
| CN106967230A (en) | 2017-07-21 |
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