CN109021562A - A kind of highly effective flame-retardant enhancing nylon composite materials and preparation method thereof - Google Patents
A kind of highly effective flame-retardant enhancing nylon composite materials and preparation method thereof Download PDFInfo
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- CN109021562A CN109021562A CN201810960525.8A CN201810960525A CN109021562A CN 109021562 A CN109021562 A CN 109021562A CN 201810960525 A CN201810960525 A CN 201810960525A CN 109021562 A CN109021562 A CN 109021562A
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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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
- 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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Abstract
The invention discloses a kind of highly effective flame-retardant enhancing nylon composite materials and preparation method thereof, are made of the component of following mass percent: nylon66 fiber 40-65%；Glass fibre 10-35%；Brominated Polystyrene 10-18%；Synergistic flame retardant 1-7%；Compatilizer 2-10%；Itaconic acid epoxy 1.5-6%；Auxiliary agent 0.5-5%；The synergistic flame retardant is one or both of antimony oxide, zinc borate.Composite material of the present invention not only has excellent anti-flammability, also has excellent mechanical property, so that solving the problems, such as to be added because of fire retardant causes the mechanical property of material and heat resistance to reduce.Composite material of the present invention realizes that preparation is simple using existing equipment double screw extruder, is easy to industrializing implementation production, has the prospect of wide application.
Description
Technical field
The present invention relates to flame retardant composite material technical fields, and in particular to a kind of highly effective flame-retardant enhancing nylon composite materials and
Preparation method.
Background technique
Nylon is polyamide, its amide group has polarity, there is firm hydrogen bond in its construction, so that
The fusing point of nylon is higher, has good mechanical property.Nylon surface hardness is big, abrasion performance, and coefficient of friction is small.Nylon has certainly
Lubricity, it is nontoxic, it is odorless, it does not go rotten, there is self-extinguishment.Nylon good weatherability, but dyeability is poor, with the miniaturization of automobile, electricity
The light-weighted progress faster of high performance, mechanical equipment of sub- electrical equipment, the demand to nylon will more Gao Geng great.Especially Buddhist nun
Dragon is used as structural material, proposes very high requirement to its anti-flammability, resistance to tracking index value (CTI) etc..
Itaconic acid epoxy is a kind of biological epoxy compound, contains carbon-carbon double bond and epoxy group, the itaconic acid epoxy
The effect for having both compatilizer and dispersing agent increases some fillers and disperses while the compatibility of matrix and inorganic additive can be improved
Property.
Therefore, it is intended that, by the good dispersibility of itaconic acid epoxy, being effectively facilitated on the basis of existing fire-retardant Nylon 66
The dispersion of fire retardant, while keeping the mechanical property of composite material.Because in most cases, the addition of fire retardant can reduce material
The mechanical property and heat resistance of material.
Authorization Notice No. is that the Chinese invention patent application of CN105694443B (application No. is 201610156718.9) is public
A kind of halogen-free flame-retardant glass fiber reinforced nylon 6 material and preparation method thereof has been opened, including following components and parts by weight content: nylon 6
50-70 parts of substrate, 5-10 parts of compound flame retardant, 0.5-1 parts of coupling agent, 0.5-1 parts of compatilizer, resists 10-20 parts of piperazine pyrophosphate
0.5-1 parts of oxygen agent and 10-30 parts of glass fibre；The compound flame retardant is hypophosphites, and the coupling agent is selected from silane
Any one in coupling agent or titanate coupling agent or two kinds, the antioxidant be 2,6- three-level butyl -4- methylphenol,
Bis- (3,5- three-level butyl -4- hydroxy phenyl) thioethers or four (β-(3,5- three-level butyl -4- hydroxy phenyl) propionic acid) pentaerythrites
Any one in ester.The technical solution improves flame retardant property by the compounding of fire retardant, but the addition of fire retardant reduces
The mechanical property and heat resistance of material.
Summary of the invention
The purpose of the present invention is to provide a kind of highly effective flame-retardant enhancing nylon composite materials and preparation method thereof, so that nylon
Composite material can have good flame retardant effect, while mechanical property with higher in a small amount of fire retardant of addition.
A kind of highly effective flame-retardant enhancing nylon composite materials, are made of the component of following mass percent:
The synergistic flame retardant is one or both of antimony oxide, zinc borate.
The present invention enhances nylon66 fiber using glass fibre, passes through flame retardant brominated polystyrene and synergistic flame retardant
The compound anti-flammability that can greatly improve composite material of antimony oxide, zinc borate, itaconic acid epoxy have both compatilizer and dispersion
The effect of agent can play obvious action to nylon and glass compatibility, the evenly dispersed of fire retardant is improved, so that of the invention
Middle each component interaction, mutually enhances, has excellent performance, not only has excellent anti-flammability, also has excellent power
Performance is learned, causes the mechanical property of material and heat resistance to reduce so as to solve the problems, such as to be added because of fire retardant.
Further preferably, the highly effective flame-retardant enhances nylon composite materials, is made of the component of following mass percent:
The synergistic flame retardant is one or both of antimony oxide, zinc borate.
Further preferably, the highly effective flame-retardant enhances nylon composite materials, is made of the component of following mass percent:
The synergistic flame retardant is one or both of antimony oxide, zinc borate.
Most preferably, the highly effective flame-retardant enhances nylon composite materials, is made of the component of following mass percent:
The synergistic flame retardant is antimony oxide.
Under the special ratios, composite material not only has excellent anti-flammability, also has excellent mechanical property,
Preferably, the weight average molecular weight of the nylon66 fiber in 18000g/mol-32000g/mol, specifically can be selected such as
BASF A27E, Du Pont 101F or first promise 21SPC, viscosity 2.6-2.7.
Preferably, 15-20 μm of the diameter of the glass fibre.
Using brominated Polystyrene as fire retardant, it can be specifically purchased from Albemarle Corporation, easy processing, excellent electrical property can
To improve the CTI value of the nylon.
Synergistic flame retardant used is antimony based compound or boron zinc compound, and antimony based compound is antimony oxide, boron zinc
Compound is zinc borate.
Preferably, compatilizer used is the ethylene-octene copolymer (POE-g-MAH) of maleic anhydride grafting.
The dispersing agent is itaconic acid epoxy, it is a kind of biological epoxy compound, has both compatilizer and dispersing agent
Effect, to improve nylon and glass compatibility, the evenly dispersed and processing performance of fire retardant has obvious action.
Preferably, auxiliary agent used be selected from one or both of antioxidant, processing aid or UV light stabilizing agent with
On, it is further preferred that antioxidant is phenols, two kinds of phosphorous acid esters.The antioxidant of phenols is the 1076 of BASF AG, phosphorous
The PEPQ of acid esters kind antioxidant Clariant company.It is further preferred that processing aid is Italy hair base PETS-AHS-AHS,
UV absorbers are the UV329 of BASF AG.
A kind of preparation method of highly effective flame-retardant enhancing nylon composite materials, method includes the following steps:
(1) by dried nylon66 fiber, flame retardant brominated polystyrene, synergistic flame retardant, compatilizer, itaconic acid epoxy and
Auxiliary agent, is added high-speed stirred pot, and revolving speed control discharges after stirring 5~15 minutes at ambient temperature, obtains in 200-500r/min
To the material mixed；
(2) material mixed is added twin-screw extrude into extruding pelletization, wherein glass fibre is from twin-screw extrusion
The extruding pelletization in double screw extruder is added in the side position material mouth of machine, obtains highly effective flame-retardant enhancing nylon composite materials.
In step (1), revolving speed is in 200-400r/min.
The preparation of the itaconic acid epoxy includes: to mix itaconic acid, epoxychloropropane and ammonium bromide in nitrogen atmosphere
Uniformly, it is warming up to 105 DEG C~120 DEG C later and maintains stirring 0.5h~2h, is gradually added dropwise after then cooling to 50 DEG C~70 DEG C
The NaOH aqueous solution of 3mol~5mol, the 3h~5h that drips after NaOH aqueous solution at 50 DEG C~70 DEG C that the reaction was continued are finally washed
Itaconic acid epoxy is obtained after drying.
The molar ratio of the itaconic acid, epoxychloropropane and ammonium bromide is 1:8~16:0.04~0.12, further excellent
Choosing, 1:12:0.08.
Further preferably, it is warming up to 110 DEG C later and maintains stirring 1h.
Further preferably, the NaOH aqueous solution that 4mol is gradually added dropwise after 60 DEG C is then cooled to.
In step (2), the revolving speed of the double screw extruder is 160-600r/min, and temperature is 180-280 DEG C.
Further preferably, the revolving speed of the double screw extruder is 160-300r/min, the double screw extruder
Each area's temperature from feed inlet to discharge port: 180-220 DEG C of area's temperature, two 230-255 DEG C of area's temperature, three area temperature 250-
260 DEG C, four 255-265 DEG C of area's temperature, five 260-270 DEG C of area's temperature, six 260-270 DEG C of area's temperature, seven area temperature 260-275
DEG C, eight 250-260 DEG C of area's temperature, 255-260 DEG C of head temperature.
Compared with prior art, the present invention has the advantage that
1. it is compound that the present invention uses common and good operability forming processing technology to prepare highly effective flame-retardant enhancing nylon
Material, the dispersing agent using the itaconic acid epoxy of biology base as fire retardant, the itaconic acid epoxy have both compatilizer and dispersing agent
Effect, to improve the compatibility of poly- nylon66 fiber and glass, the evenly dispersed and processing performance of fire retardant has significant make
With.
2. highly effective flame-retardant enhancing nylon composite materials described in can reach V-0 grades of resistance when flame retardant agent content is less
Fuel efficiency fruit, and mechanical property is kept preferably, excellent combination property.
Specific embodiment
The present invention is specifically described below by embodiment, it is necessary to which indicated herein is that following embodiment is served only for
Invention is further explained, should not be understood as limiting the scope of the invention, the person skilled in the art in the field
Some nonessential modifications and adaptations are made to the present invention according to aforementioned present invention.
Preparation example
The preparation of itaconic acid epoxy:
The ammonium bromide of the itaconic acid of 1mol, the epoxychloropropane of 12mol and 0.08mol is added in round-bottomed flask, is passed through
Nitrogen atmosphere stirs 0.5h at 25 DEG C of room temperature, and uses mechanical stirring.It is gradually warming up to 110 DEG C afterwards and maintains stirring 1h, cooling
The NaOH aqueous solution of 4mol is gradually added dropwise after to 60 DEG C, the 4h that drips after NaOH at 60 DEG C that the reaction was continued finally uses polymer
Deionized water settles out, and filters cleaning 3 times, and it is stand-by that drying obtains itaconic acid epoxide resin afterwards for 24 hours.
Embodiment 1
(1) by nylon66 fiber (PA66, BASF A27E, weight average molecular weight is in 18000g/mol-32000g/mol) in air blast
Drying will be in 120 DEG C of vacuum drying 4h, by dried PA66, glass fibre (15-20 μm of glass diameter), brominated Polystyrene
(Albemarle Corporation), antimony oxide, zinc borate, POE-g-MAH (ethylene-octene copolymer of maleic anhydride grafting, Dow
GR216), preparation example preparation itaconic acid epoxy, antioxidant 1076 (BASF AG), antioxidant PEPQ (Clariant company),
The mass percent of processing aid PETS-AHS (Italy hair base PETS-AHS), UV absorbers UV329 (BASF AG)
As shown in table 1.It is mixed 10 minutes in 80 DEG C of high mixers using 300rpm, obtains mixture；
(2) by mixture extruding pelletization in double screw extruder obtained by step (1), it is multiple to obtain highly effective flame-retardant enhancing nylon
Condensation material.Each area's temperature (from feed inlet to discharge port) of double screw extruder and screw speed are respectively as follows: area's temperature 220
DEG C, two 250 DEG C of area's temperature, three 250 DEG C of area's temperature, four 260 DEG C of area's temperature, five 270 DEG C of area's temperature, six 270 DEG C of area's temperature, 7th area
275 DEG C of temperature, eight 260 DEG C of area's temperature, 260 DEG C of head temperature；Screw speed is 200r/min.
Embodiment 2
Formula composition is same as Example 1, and mass percent is different, as shown in table 1.Temperature unlike in processing method
And screw speed, wherein each area's temperature and screw speed are respectively as follows: 210 DEG C of area's temperature, two 245 DEG C of area's temperature, three area's temperature
250 DEG C, four 260 DEG C of area's temperature, five 270 DEG C of area's temperature, six 270 DEG C of area's temperature, seven 275 DEG C of area's temperature, eight 260 DEG C of area's temperature,
260 DEG C of head temperature；Screw speed is 280r/min.
Embodiment 3
Formula composition is same as Example 1, and mass percent is different, as shown in table 1.Temperature unlike in processing method
And screw speed, wherein each area's temperature and screw speed are respectively as follows: 200 DEG C of area's temperature, two 240 DEG C of area's temperature, three area's temperature
250 DEG C, four 260 DEG C of area's temperature, five 270 DEG C of area's temperature, six 270 DEG C of area's temperature, seven 275 DEG C of area's temperature, eight 260 DEG C of area's temperature,
260 DEG C of head temperature；Screw speed is 300r/min.
Embodiment 4
Formula composition is same as Example 1, and mass percent is different, as shown in table 1.Temperature unlike in processing method
And screw speed, wherein each area's temperature and screw speed are respectively as follows: 185 DEG C of area's temperature, two 235 DEG C of area's temperature, three area's temperature
250 DEG C, four 255 DEG C of area's temperature, five 265 DEG C of area's temperature, six 265 DEG C of area's temperature, seven 265 DEG C of area's temperature, eight 255 DEG C of area's temperature,
255 DEG C of head temperature；Screw speed is 400r/min.
Comparative example 1:
Comparative example 1 does not use itaconic acid epoxy, remaining is with embodiment 1, and see Table 1 for details for concrete component and mass percent, system
Preparation Method is same as Example 1.
Comparative example 2:
Comparative example 2 does not use flame retardant brominated polystyrene, and, with embodiment 1, concrete component and mass percent are detailed for remaining
It is shown in Table 1, preparation method is same as Example 1.
Comparative example 3:
Comparative example 3 does not use synergistic flame retardant antimony oxide, remaining is the same as embodiment 1, concrete component and mass percent
See Table 1 for details, and preparation method is same as Example 1.
By the resulting composite material pellet of above-described embodiment 1-4 and comparative example 1-3, distribution is molded by national standard, related
Testing standard is as follows:
Tensile property test: GB/T 1040-2006；
Bending property test: GB/T 9341-2000；
Izod notched impact: GB/T 1843-2008；
Heat resistance (HDT) test: GB/T 1634-2004；
Flame retardant property test: GB/T 2408-2008；
CTI (resistance to electric leakage trace index value) test: GB/T 4207-2003.
Table 1 is the mass percent of each component substance in embodiment 1-4 and comparative example 1-3, and table 2 is embodiment 1-4 and right
The performance test results of resulting materials in ratio 1-3.
Table 1
Table 2
As can be seen from Table 1 and Table 2, comparative example 1 does not use itaconic acid epoxy, and comparative example 1 passes through addition brominated polyphenylene second
Alkene and antimony oxide can greatly improve the flame retardant property of composite material, and have high CTI (relative discharge tracking index)
Value, but due to the addition of brominated Polystyrene and antimony oxide, composite materials property is caused to reduce, embodiment 1 is adopted
The anti-flammability of composite material can be greatly improved by addition brominated Polystyrene and antimony oxide with itaconic acid epoxy
Can, and there is high CTI (relative discharge tracking index) value, simultaneously as the addition of itaconic acid epoxy, each component can be preferably
It is fused together, makes it have excellent mechanical property.Comparative example 2 does not use flame retardant brominated polystyrene, flame retardant property
It is poor, standard is not achieved, CTI (relative discharge tracking index) value also only has 200.Comparative example 3 does not use three oxygen of synergistic flame retardant
Change two antimony, flame retardant property reaches V-1, CTI (relative discharge tracking index) value lower 260.As it can be seen that fire-retardant in embodiment 1-4
For PA66 composite material while with excellent fire-retardancy, mechanical property is also fine.Illustrate, the addition of itaconic acid epoxy can
Effectively to disperse fire retardant, and increase the interface between PA66 and glass, maintain PA66 composite material flame retardant property and
Mechanical property.Itaconic acid epoxy has both the effect of compatilizer and dispersing agent, to improve nylon and glass compatibility, fire retardant it is equal
Even dispersion can play obvious action, so that each component interacts in the present invention, mutually enhance, have excellent performance,
Not only there is excellent anti-flammability, also there is excellent mechanical property, so as to solve because fire retardant addition leads to material
Mechanical property and heat resistance reduce the problem of.
Claims (10)
1. a kind of highly effective flame-retardant enhances nylon composite materials, which is characterized in that be made of the component of following mass percent:
The synergistic flame retardant is one or both of antimony oxide, zinc borate.
2. highly effective flame-retardant according to claim 1 enhances nylon composite materials, which is characterized in that by following mass percent
Component be made:
The synergistic flame retardant is one or both of antimony oxide, zinc borate.
3. highly effective flame-retardant according to claim 1 enhances nylon composite materials, which is characterized in that by following mass percent
Component be made:
The synergistic flame retardant is one or both of antimony oxide, zinc borate.
4. highly effective flame-retardant according to claim 1,2 or 3 enhances nylon composite materials, which is characterized in that used is compatible
Agent is the ethylene-octene copolymer of maleic anhydride grafting.
5. the preparation method of highly effective flame-retardant enhancing nylon composite materials according to any one of claims 1 to 4, feature exist
In, method includes the following steps:
(1) dried nylon66 fiber, brominated Polystyrene, synergistic flame retardant, compatilizer, itaconic acid epoxy and auxiliary agent are pressed, is added
High-speed stirred pot, revolving speed control discharge after stirring 5~15 minutes at ambient temperature, are mixed in 200-500r/min
Material；
(2) material mixed is added twin-screw extrude into extruding pelletization, wherein glass fibre is from double screw extruder
The extruding pelletization in double screw extruder is added in side position material mouth, obtains highly effective flame-retardant enhancing nylon composite materials.
6. preparation method according to claim 5, which is characterized in that in step (1), in step (1), revolving speed is in 200-
400r/min。
7. preparation method according to claim 5, which is characterized in that in step (1), the preparation of the itaconic acid epoxy
Include: to be uniformly mixed itaconic acid, epoxychloropropane and ammonium bromide in nitrogen atmosphere, is warming up to 105 DEG C~120 DEG C later and ties up
Stirring 0.5h~2h is held, the NaOH aqueous solution of 3mol~5mol is gradually added dropwise after then cooling to 50 DEG C~70 DEG C, drips
The reaction was continued at 50 DEG C~70 DEG C after NaOH aqueous solution 3h~5h obtains itaconic acid epoxy after finally washing is dry.
8. preparation method according to claim 7, which is characterized in that itaconic acid, epoxychloropropane and the ammonium bromide
Molar ratio be 1:8~16:0.04~0.12.
9. preparation method according to claim 5, which is characterized in that in step (2), the double screw extruder turns
Speed is 160-600r/min, and temperature is 180-280 DEG C.
10. preparation method according to claim 9, which is characterized in that in step (2), the double screw extruder
Revolving speed is 160-300r/min, each area temperature of the double screw extruder from feed inlet to discharge port: an area temperature 180-
220 DEG C, two 230-255 DEG C of area's temperature, three 250-260 DEG C of area's temperature, four 255-265 DEG C of area's temperature, five area temperature 260-270
DEG C, six 260-270 DEG C of area's temperature, seven 260-275 DEG C of area's temperature, eight 250-260 DEG C of area's temperature, 255-260 DEG C of head temperature.
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| CN112552680A (en) * | 2020-12-11 | 2021-03-26 | 上海金发科技发展有限公司 | Efficient flame-retardant nylon composite material and preparation method thereof |
| CN115584123A (en) * | 2022-10-09 | 2023-01-10 | 江西金石三维智能制造科技有限公司 | Reinforced nylon composite material for printer and preparation method thereof |
| CN116694072A (en) * | 2023-07-13 | 2023-09-05 | 苏州优利金新材料有限公司 | High-flame-retardance nylon composite material and preparation method thereof |
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| CN116694072B (en) * | 2023-07-13 | 2023-11-28 | 苏州优利金新材料有限公司 | High-flame-retardance nylon composite material and preparation method thereof |
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| CN109021562B (en) | 2020-11-06 |
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