CN108948476A - A kind of halogen-free fire-retardant polyethylene material and preparation method thereof - Google Patents
A kind of halogen-free fire-retardant polyethylene material and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C08L2201/22—Halogen free composition
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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- C—CHEMISTRY; METALLURGY
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- C08L2207/00—Properties characterising the ingredient of the composition
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Abstract
The invention belongs to technical field of polymer materials, it is related to a kind of halogen-free polythene flame redardant composite material, its raw materials for production comprises the following components in parts by weight: 35-45 parts of polyvinyl resin, 10-20 parts of acrylic resin, 35-40 parts of halogen-free flame retardants, 0.4-0.6 parts of antioxidant, 0.5-1.0 parts of lubricant, 2-5 parts of compatilizer, 3-5 parts of toughener.The invention further relates to the preparation methods of halogen-free polythene flame redardant composite material.Preparation process of the present invention is simple, and gained composite material is both with good anti-flammability and mechanical property.
Description
Technical field
The invention belongs to technical field of polymer materials, it is related to a kind of halogen-free fire-retardant polyethylene material and preparation method thereof.
Background technique
Polyethylene (PE) has superior electrical insulating property, chemical corrosion resistance and cold resistance, and nontoxic, light, valence
Lattice are cheap, are widely used in the industries such as daily packaging, building, communications and transportation, wire and cable, wherein being widely used in cable electricity
Gas industry, the sector is to flame-retardancy requirements height, but the oxygen index (OI) of PE is 17.5, belongs to inflammable high molecular material, so being applied to
The polythene material of electric utility is required by flame-retardant modified.
PE fire-retardant early stage is the method for compounding addition with antimony oxide using halogen system object, and this method flame retarding efficiency is high, but
A large amount of smog and toxic, mordant gas can be released when being the fire-retardant PE material combustion of halogen system object, environment is caused
Pollution, damages the person.Currently, greatly developing Non-halogen Flame Retardant Technology both at home and abroad, that is, add inorganic hydroxide, this kind of resistance
Combustion agent, which decomposes heat absorption and decomposes the water dilution combustible generated, reaches fire-retardant purpose, the disadvantage is that additive amount is big, generally 50% with
On, the mechanical property and processing performance that will lead to material in this way are decreased obviously；Or addition expansion type flame retardant, the fire retardant are logical
It crosses and is formed uniform expansion carbon-coating on the surface of the material by thermal decomposition, reach flame retardant effect, fire-retardant effect by the modes such as heat-insulated, oxygen barrier
Rate is compared with hydroxide height, and application is than wide now.
Expansion type flame retardant is generally by acid source (ammonium polyphosphate, melamine polyphosphates), gas source (melamine), carbon source (season
Penta tetrol) it is mixed to get in proportion, the flame retarding efficiency of this fire retardant is high, but the poor compatibility with PE, and fire retardant is easy analysis
Surface is easy to appear the case where whitening when out and being made into colored article, has seriously affected the use scope of fire-retardant PE material.
Summary of the invention
A kind of Zero halogen flame resistance polyethylene material is provided it is an object of the invention to overcome the problems of the above-mentioned prior art
Material, a kind of halogen-free fire-retardant polyethylene material avoid while with good flame-retardance due to fire retardant and PE compatibility
When colored article being made caused by difference, surface is easy the case where whitening.
It is a further object to provide a kind of preparation methods of halogen-free fire-retardant polyethylene material.
To achieve the above object, the invention adopts the following technical scheme:
A kind of halogen-free polythene flame redardant composite material, raw materials for production comprise the following components in parts by weight:
The polyvinyl resin is high density polyethylene (HDPE) (HDPE), melts and refers to the 0.5-5g/10min (test condition of melting means
It is 190 DEG C, 2.16Kg).
The acrylic resin is copolymer polypropylene.
The halogen-free flame retardants is nitrogen phosphorus system expanding fire retardant；Preferably, the halogen-free flame retardants is by ammonium polyphosphate, trimerization
The mixture of cyanamide and pentaerythrite, weight ratio 3-5:1-5:1-3.
The antioxidant is by four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters (antioxidant 1010)
It is formed with three [2.4- di-tert-butyl-phenyl] phosphite esters (irgasfos 168)；Preferably, four [β-(3, the 5- di-t-butyls-
4- hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010) and three [2.4- di-tert-butyl-phenyl] phosphite ester (antioxidant
168) composition ratio is 1:1-1:2.
The lubricant be one of calcium stearate, polyethylene wax, ethylene bis stearamide (EBS) and silicone with
On.
The compatilizer is in maleic anhydride inoculated polypropylene (PP-G) and ethylene-vinyl acetate copolymer (EVA)
More than one；Preferably, the content of vinylacetate is 15-25% in the EVA.
The toughener is polyolefin elastomer (POE).
The raw materials for production of the composite polyethylene material further include toner；Preferably, the number of the toner is pigment
Red 226.
The invention also discloses a kind of preparation methods of halogen-free polythene flame redardant composite material, comprising the following steps:
It (1) is 35-45 parts of polyvinyl resin, 10-20 parts of acrylic resin, the resistance of 35-40 parts of Halogen by parts by weight
Fire agent, 0.4-0.6 parts of antioxidant, 0.5-1.0 parts of lubricant, 2-5 parts of compatilizer, 3-5 parts of toughener, 0-4 parts
Toner is uniformly mixed in a high speed mixer, obtains mixture；
(2) mixture obtained by step (1), which enters, carries out melting mixing in double screw extruder, squeeze out, and cooling, is done pelletizing
After dry step, halogen-free polythene flame redardant composite material can be obtained.
High mixer revolving speed is 500-800rpm, incorporation time 3-10min in the step (1).
The temperature in each area of double screw extruder is 180 DEG C~220 DEG C in the step (2).
Compared with prior art, the present invention has the advantage that
(1) products obtained therefrom keeps its various function mutually auxiliary by the way that polypropylene, fire retardant and lubricant silicone is added in the present invention
It coordinates, coordinated, when to reach avoiding that colored article is made caused by due to fire retardant and PE poor compatibility, surface is easy
The case where whitening is that product has good surface property, and has excellent toughness, has widened the application range of the product.
(2) products obtained therefrom has reached phase in the case where reducing flame retardant agent content by the way that polypropylene is added in the present invention
With combustion rating, also avoid caused by the increase due to fire retardant additive amount under product mechanical property and processing performance
Drop.
Specific embodiment
The present invention will be further described by the following examples,
Test method of the present invention to following comparative examples and each performance of embodiment are as follows:
Tensile strength test method: ASTM D638-039；
Notch impact strength test method: ASTM D256；
Flame retardant property standard uses: UL-94.
Embodiment 1
It (1) is 35 parts of high-density polyethylene resin, 20 parts of acrylic resin copolymer, the resistance of 35 parts of Halogen by parts by weight
Fire agent (ammonium polyphosphate, melamine and pentaerythrite weight ratio 4:2:2), 0.4 part of antioxidant (four [β-(3,5- bis- tertiary fourths
Base -4- hydroxy phenyl) propionic acid] pentaerythritol ester and three [2.4- di-tert-butyl-phenyl] phosphite ester weight ratio 1:1), 0.2 part
Polyethylene wax, 0.3 part of silicone, 5 parts of PP-G, 5 parts of POE are uniformly mixed in a high speed mixer, obtain mixture, and height is mixed
Machine revolving speed is 500rpm, incorporation time 10min；
(2) mixture obtained by step (1), which enters, carries out melting mixing in double screw extruder, squeeze out, and cooling, is done pelletizing
Dry, the temperature in each area of double screw extruder is 180 DEG C~220 DEG C, can be obtained halogen-free polythene flame redardant composite material.Gained is multiple
Condensation material is tested, and properties are shown in Table 2.
Embodiment 2
It (1) is 40 parts of high-density polyethylene resin, 15 parts of acrylic resin copolymer, the resistance of 37 parts of Halogen by parts by weight
Fire agent (ammonium polyphosphate, melamine and pentaerythrite weight ratio 5:3:2), 0.5 part of antioxidant (four [β-(3,5- bis- tertiary fourths
Base -4- hydroxy phenyl) propionic acid] pentaerythritol ester and three [2.4- di-tert-butyl-phenyl] phosphite ester weight ratio 1:1), 0.3 part
Calcium stearate, 0.5 part of silicone, 5 parts of EVA (content of vinylacetate is 20%), 3 parts of POE, 4 parts of paratonere 226
It is uniformly mixed in a high speed mixer, obtains mixture, high mixer revolving speed is 500rpm, incorporation time 10min；
(2) mixture obtained by step (1), which enters, carries out melting mixing in double screw extruder, squeeze out, and cooling, is done pelletizing
Dry, the temperature in each area of double screw extruder is 180 DEG C~220 DEG C, can be obtained halogen-free polythene flame redardant composite material.Gained is multiple
Condensation material is tested, and properties are shown in Table 2.
Embodiment 3
It (1) is 42 parts of high-density polyethylene resin, 10 parts of acrylic resin copolymer, the resistance of 38 parts of Halogen by parts by weight
Fire agent (ammonium polyphosphate, melamine and pentaerythrite weight ratio 3:1:3), 0.5 part of antioxidant (four [β-(3,5- bis- tertiary fourths
Base -4- hydroxy phenyl) propionic acid] pentaerythritol ester and three [2.4- di-tert-butyl-phenyl] phosphite ester weight ratio 1:1), 0.5 part
Polyethylene wax, 0.5 part of silicone, 5 parts of PP-G, 5 parts of POE, 1 part of paratonere 226 are uniformly mixed in a high speed mixer,
Mixture is obtained, high mixer revolving speed is 700rpm, incorporation time 5min；
(2) mixture obtained by step (1), which enters, carries out melting mixing in double screw extruder, squeeze out, and cooling, is done pelletizing
Dry, the temperature in each area of double screw extruder is 180 DEG C~220 DEG C, can be obtained halogen-free polythene flame redardant composite material.Gained is multiple
Condensation material is tested, and properties are shown in Table 2.
Embodiment 4
It (1) is 45 parts of high-density polyethylene resin, 10 parts of acrylic resin copolymer, the resistance of 40 parts of Halogen by parts by weight
Fire agent (ammonium polyphosphate, melamine and pentaerythrite weight ratio 4:2:2), 0.6 part of antioxidant (four [β-(3,5- bis- tertiary fourths
Base -4- hydroxy phenyl) propionic acid] pentaerythritol ester and three [2.4- di-tert-butyl-phenyl] phosphite ester weight ratio 1:2), 0.5 part
Polyethylene wax, 0.5 part of silicone, 2 parts of PP-G, 3 parts of POE are uniformly mixed in a high speed mixer, obtain mixture, and height is mixed
Machine revolving speed is 800rpm, incorporation time 3min；
(2) mixture obtained by step (1), which enters, carries out melting mixing in double screw extruder, squeeze out, and cooling, is done pelletizing
Dry, the temperature in each area of double screw extruder is 180 DEG C~220 DEG C, can be obtained halogen-free polythene flame redardant composite material.Gained is multiple
Condensation material is tested, and properties are shown in Table 2.
Comparative example 1
It (1) is 55 parts of polyvinyl resin, 40 parts of halogen-free flame retardants (ammonium polyphosphate, melamine and season by parts by weight
Penta tetrol weight ratio 4:2:2), 0.6 part antioxidant (four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythrites
Ester and three [2.4- di-tert-butyl-phenyl] phosphite ester weight ratio 1:2), 0.5 part of polyethylene wax, 0.5 part of silicone, 5 parts
POE is uniformly mixed in a high speed mixer, obtains mixture, and high mixer revolving speed is 800rpm, incorporation time 3min；
(2) mixture obtained by step (1), which enters, carries out melting mixing in double screw extruder, squeeze out, and cooling, is done pelletizing
Dry, the temperature in each area of double screw extruder is 180 DEG C~220 DEG C, can be obtained halogen-free polythene flame redardant composite material.Gained is multiple
Condensation material is tested, and properties are shown in Table 2.
Comparative example 2
It 1) is 40 parts of polyvinyl resin, 15 parts of acrylic resin, 37 parts of halogen-free flame retardants (polyphosphoric acid by parts by weight
Ammonium, melamine and pentaerythrite weight ratio 5:3:2), 0.5 part of antioxidant (four [β-(3,5- di-t-butyl -4- hydroxy benzenes
Base) propionic acid] pentaerythritol ester and three [2.4- di-tert-butyl-phenyl] phosphite ester weight ratio 1:1), 0.3 part of calcium stearate, 5
The EVA (content of vinylacetate is 20%), 3 parts of POE of part are uniformly mixed in a high speed mixer, obtain mixture, high
Mixed machine revolving speed is 500rpm, incorporation time 10min；
(2) mixture obtained by step (1), which enters, carries out melting mixing in double screw extruder, squeeze out, and cooling, is done pelletizing
Dry, the temperature in each area of double screw extruder is 180 DEG C~220 DEG C, can be obtained halogen-free polythene flame redardant composite material.Gained is multiple
Condensation material is tested, and properties are shown in Table 2.
The parts by weight list 1 of above-described embodiment 1 to 4 and each component of comparative example 1 and 2.
Table 1
| Raw material | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 |
| HDPE | 35 | 40 | 42 | 45 | 55 | 40 |
| Copolymer polypropylene | 20 | 15 | 10 | 10 | / | 15 |
| Fire retardant | 35 | 37 | 38 | 40 | 40 | 37 |
| Antioxidant | 0.4 | 0.5 | 0.5 | 0.6 | 0.6 | 0.5 |
| Polyethylene wax | 0.2 | / | 0.5 | 0.5 | 0.5 | 0.5 |
| Calcium stearate | / | 0.3 | / | / | / | 0.3 |
| Silicone | 0.3 | 0.5 | 0.5 | 0.5 | 0.5 | / |
| PP-G | 5 | / | 5 | 2 | / | / |
| EVA | / | 5 | / | / | / | 5 |
| POE | 5 | 3 | 5 | 3 | 5 | 3 |
| Paratonere 226 | / | 4 | 1 | / | / | / |
The mechanical experimental results of embodiment 1-4 and the gained composite material of comparative example 1 and 2 such as table 2.
Table 2
| Performance | Unit | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 |
| Tensile strength | MPa | 16.6 | 16.1 | 15.4 | 15.2 | 17.0 | 15.8 |
| Notch shock | KJ/m2 | 13 | 12 | 15 | 12 | 10 | 12 |
| Flame retardant property | / | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 |
| Surface property | / | It is excellent | It is good | It is good | It is good | Whiten serious | It is good |
It follows that 1) polyacrylic addition from the test result of table 2, so that material surface property improves, it is seen that poly-
The compatibility of propylene and expansion type flame retardant is preferable；2) polyacrylic addition can also be reached in the case where reducing flame retardant agent content
To identical combustion rating；3) polyacrylic be added influences less the toughness of material；4) difference of comparative example 2 and embodiment 2
It is that lubricant uses polyethylene wax and silicone respectively, two samples is placed in 100 DEG C of baking oven and are heated, places one
Section the time after plus silicone sample surfaces occur white tacky substance, added silicone product surface or bright and clean, explanation
Lubricant silicone is precipitated with positive effect to prevent fire retardant.The material can be used for expanding surface requirements high color product
The big application range of expansion type flame-retarding PE.
The above-mentioned description to embodiment is for that can understand and apply the invention convenient for those skilled in the art.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to embodiments here, originally
Field technical staff announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be in the present invention
Protection scope within.
Claims (10)
1. a kind of halogen-free polythene flame redardant composite material, it is characterised in that: its raw materials for production comprises the following components in parts by weight:
2. composite polyethylene material according to claim 1, it is characterised in that: the polyvinyl resin is high-density polyethylene
Alkene.
3. composite polyethylene material according to claim 1, it is characterised in that: the acrylic resin is copolymerization poly- third
Alkene.
4. composite polyethylene material according to claim 1, it is characterised in that: the halogen-free flame retardants is the expansion of nitrogen phosphorus system
Fire retardant；
Preferably, nitrogen phosphorus system's expanding fire retardant is the mixture of ammonium polyphosphate, melamine and pentaerythrite, weight ratio
For 3-5:1-5:1-3.
5. composite polyethylene material according to claim 1, it is characterised in that: the antioxidant is by four [β-(3,5- bis- uncles
Butyl -4- hydroxy phenyl) propionic acid] pentaerythritol ester and three [2.4- di-tert-butyl-phenyl] phosphite esters form；
Preferably, four [β-(3, the 5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester and three [2.4- di-t-butyls
Phenyl] phosphite ester composition ratio be 1:1-1:2.
6. composite polyethylene material according to claim 1, it is characterised in that: the lubricant is calcium stearate, poly- second
One or more of alkene wax, ethylene bis stearamide and silicone.
7. composite polyethylene material according to claim 1, it is characterised in that: the compatilizer is that maleic anhydride grafting is poly-
One or more of propylene and ethylene-vinyl acetate copolymer；
Preferably, vinyl acetate content is 15-25% in ethylene-vinyl acetate copolymer；
Preferably, the toughener is polyolefin elastomer.
8. composite polyethylene material according to claim 1, it is characterised in that: the raw materials for production of the composite polyethylene material
It further include the toner that parts by weight are 0-4 parts；
Preferably, the number of the toner is paratonere 226.
9. a kind of preparation method of halogen-free polythene flame redardant composite material, it is characterised in that: the following steps are included:
(1) by parts by weight be 35-45 parts of polyvinyl resin, 10-20 parts of acrylic resin, 35-40 parts of halogen-free flame retardants,
0.4-0.6 parts of antioxidant, 0.5-1.0 parts of lubricant, 2-5 parts of compatilizer, 3-5 parts of toughener are in a high speed mixer
It is uniformly mixed, obtains mixture；
(2) mixture obtained by step (1) carries out melting mixing from double screw extruder, squeezes out, cooling, pelletizing, drying steps
Afterwards, it can be obtained halogen-free polythene flame redardant composite material.
10. the preparation method of composite material as claimed in claim 9, it is characterised in that: step (1) the high speed mixing machine
Revolving speed is 500-800rpm, incorporation time 3-10min；
Preferably, the temperature in each area of double screw extruder is 180 DEG C~220 DEG C in the step (2).
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| CN112143082A (en) * | 2020-10-10 | 2020-12-29 | 刘小龙 | High-strength flame-retardant PE material and preparation method thereof |
| CN112300465A (en) * | 2019-07-24 | 2021-02-02 | 中国石油天然气股份有限公司 | Polyethylene resin composition |
| CN112646257A (en) * | 2020-12-29 | 2021-04-13 | 无锡鸿仪新材料科技有限公司 | High-density polyethylene sheath material and preparation process thereof |
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| CN109705462A (en) * | 2018-12-25 | 2019-05-03 | 广东聚石化学股份有限公司 | A kind of dedicated V0 grade halogen-free flame-retardant polypropylene material of extrusion plastic uptake and preparation method thereof |
| CN109705462B (en) * | 2018-12-25 | 2021-08-24 | 广东聚石化学股份有限公司 | V0-grade halogen-free flame-retardant polypropylene material special for extrusion and plastic uptake and preparation method thereof |
| CN110079008A (en) * | 2019-01-21 | 2019-08-02 | 池州市锐强新材料有限公司 | A kind of halogen-free intumescent flame-retardant special breathable membrane material and preparation method thereof |
| CN112300465A (en) * | 2019-07-24 | 2021-02-02 | 中国石油天然气股份有限公司 | Polyethylene resin composition |
| CN112143082A (en) * | 2020-10-10 | 2020-12-29 | 刘小龙 | High-strength flame-retardant PE material and preparation method thereof |
| CN112646257A (en) * | 2020-12-29 | 2021-04-13 | 无锡鸿仪新材料科技有限公司 | High-density polyethylene sheath material and preparation process thereof |
| CN114957826A (en) * | 2021-02-26 | 2022-08-30 | 合肥杰事杰新材料股份有限公司 | Extrusion-grade halogen-free flame-retardant wood-plastic composite material and preparation method and application thereof |
| CN113462052A (en) * | 2021-06-08 | 2021-10-01 | 太仓市华旭塑胶科技有限公司 | Flame-retardant garbage can made of composite polymer material and preparation method |
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