CN109705571A - A kind of low-density, low smell bromine system flame-retardant reinforced nylon 66 and preparation method thereof - Google Patents
A kind of low-density, low smell bromine system flame-retardant reinforced nylon 66 and preparation method thereof Download PDFInfo
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- CN109705571A CN109705571A CN201811584702.3A CN201811584702A CN109705571A CN 109705571 A CN109705571 A CN 109705571A CN 201811584702 A CN201811584702 A CN 201811584702A CN 109705571 A CN109705571 A CN 109705571A
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Abstract
The present invention relates to nylon field, in particular to a kind of low-density, low smell bromine system flame-retardant reinforced nylon 66 and preparation method thereof.Wherein, low-density, low smell bromine system flame-retardant reinforced nylon 66 are made of the component that following parts by weight match: 49 parts -69.5 parts of PA66 resin, 15 parts -30 parts of glass fibre, 10 parts -12 parts of bromide fire retardant, 3 parts -5 parts of expanded graphite, 2 parts -3 parts of antimony oxide, 0.5 part -1 part of processing aid.A kind of low-density provided by the invention, low smell bromine system flame-retardant reinforced nylon 66 have lower density and smell, can be used in has in the product of strict demand smell, lightweight compared with the conventional fire-retardant reinforced plastic PA66 of bromine system.
Description
Technical field
The present invention relates to nylon field, in particular to a kind of low-density, low smell bromine system flame-retardant reinforced nylon 66 and its system
Preparation Method.
Background technique
Nylon66 fiber (abbreviation PA66) is milky semi-crystalline polymer, it has, and thermodynamic property is excellent, heat-resisting, rub system
Number is low, wear-resistant, self-lubrication is good, also has many advantages, such as oil resistant, weak acid resistant, electrical insulating property are good, is widely used in electronics electricity
The fields such as device, automobile, machinery are that yield is big in polyamide family, one of widely used kind.In terms of fire-retardant nylon, mesh
Preceding apply can be divided into bromine system, phosphorus system, nitrogen system, inorganic hydroxide, borate etc. in effective fire retardant of PA66, wherein again with bromine
It is that fire-retardant dosage is maximum, it is the advantages that this is that flame-retardant PA 66 has good flame resistance, at low cost, good mechanical property, easy processing, extensive
It applies on the products such as electric power connector, electric switch, breaker, motor accessory, charging pile accessory.With automobile mechanical and electricity
The development of sub- electrical apparatus industry, the improvement of people's living standards, each field put forward higher requirements the application of flame-retardant PA 66 material,
The high-performance of material, lightweight, low smell, environmental protection become new trend.And bromine system flame-retardant PA 66 smell is big, smoke amount is high, nothing
Method applies the component for having strict demand to smell in automobile interior decoration etc..
Summary of the invention
To solve the problems, such as to mention in above-mentioned background technique, the present invention provides a kind of low-density, the fire-retardant increasing of low smell bromine system
Strong nylon66 fiber and preparation method thereof, wherein low-density, low smell bromine system flame-retardant reinforced nylon 66 are matched by following parts by weight
Component is constituted:
Further, the PA66 resin is adipic acid and the polyamide 66 resin that hexamethylene diamine polycondensation reaction obtains；It is described
The fusing point of PA66 resin is 250-270 DEG C, relative viscosity 2.0-3.0.
Further, the bromide fire retardant be brominated polystyrene, brominated Polystyrene, in decabromodiphenylethane at least
It is a kind of.
Further, the glass fibre is alkali-free chopped strand；The diameter of the glass fibre is 10-14 μm, length
For 3-4.5mm.
Further, the phosphorus content ﹥ 99.5% of the expanded graphite, partial size are 12-14 μm.
Further, the processing aid be one of primary antioxidant, auxiliary anti-oxidant, in-lubricant and external lubricant or
Two or more combinations.
Low-density provided by the invention, low smell bromine system flame-retardant reinforced nylon 66, pass through PA66 resin and expanded graphite, bromine
The synergistic effect of flame retardant and antimony oxide, greatly reduces the dosage of bromide fire retardant, and has reached excellent fire-retardant
Effect；Realize the density for reducing material and odor profiles purpose.A kind of low-density provided by the invention, the resistance of low smell bromine system
Reinforced PA66 is fired, compared with the conventional fire-retardant reinforced plastic PA66 of bromine system, there is lower density and smell, can be used in gas
Taste, lightweight have in the product of strict demand.
The present invention additionally provides a kind of low-density, the preparation method of low smell bromine system flame-retardant reinforced nylon 66, using taking up an official post
The meaning low-density, low smell bromine system flame-retardant reinforced nylon 66, the preparation method is specific as follows:
S10, PA66 resin is dried into 80-90 DEG C of dehumidifying device 4-6h, controls moisture less than 0.2%；
It is S20, dried PA66 resin, processing aid and expanded graphite is pre- in high mixer high speed according to the weight ratio
Mixed 2-5min；
After the completion of S30, premix, bromide fire retardant, synergistic flame retardant are added according to the weight ratio, it is equal to continue to use high mixer
It is mixed, until each component is uniformly mixed；
Extruder is sent into S40, the raw material that step S30 is mixed, discharging, carries out fusion plastification, kneading mixing, and alkali-free is short
Cut fiber and be added through Weightlessness balance by side feed material, most afterwards through head extrusion, tie rod, cooling, pelletizing, drying, can be obtained low-density,
66 material of low smell bromine system flame-retardant reinforced nylon.
Further, the draw ratio of extruder described in step S40 is 44:1, and extruder temperature is 220-280 DEG C, screw rod
Revolving speed is 300-600rpm.
Preparation method provided by the invention has prepared low-density, low smell bromine system by the collaboration between each step
Flame-retardant reinforced nylon 66.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
It is clearly and completely described, it is clear that described embodiments are some of the embodiments of the present invention, rather than whole implementation
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
The present invention provides following examples, and each embodiment component is as shown in table 1:
Table 1
The processing aid be one or both of primary antioxidant, auxiliary anti-oxidant, in-lubricant and external lubricant with
On combination.Wherein, the antioxidant is the compound or amine of Hinered phenols antioxidant and phosphite ester antioxidant
The compound of antioxidant and phosphite ester antioxidant.The lubricant is E wax, calcium stearate, silicone master batch or season penta
One of tetrol stearate or two or more compositions.
Each embodiment is prepared via a method which:
Embodiment 1
S10,69 parts of PA66 resins are dried into 80 DEG C of dehumidifying device 6h, controls moisture less than 0.2%；The step
Middle PA66 resin uses polyamide 66 resin, polyamide 66 resin heat resistance with higher and cost performance.Wherein, PA66 resin
Fusing point be 260 DEG C, relative viscosity 2.0；If it is inadequate that fusing point crosses low heat resistant, excessive price is high；Also, PA66 resin exists
Its mobility and processability are best within the scope of 2.0-3.0.
S20, by dried PA66 resin, 0.2 part of primary antioxidant, 0.3 part of in-lubricant 0 and 5 part expanded graphite according to
Weight proportion premixes 5min in high mixer high speed；In the step, the phosphorus content ﹥ 99.5% of expanded graphite, partial size is 13 μm；It is swollen
Swollen graphite phosphorus content with higher, with fire retardant rise synergistic effect when, carbon forming rate is higher, can preferably play it is oxygen barrier every
The effect of heat, becomes apparent from fire-retardant effect, therefore can reduce the dosage of bromide fire retardant；Because bromide fire retardant density is big, drop
Low bromide fire retardant dosage is equivalent to the density for reducing material.It is best when by expanded graphite partial size being 13 μm, it is too small then swollen
Swollen graphite is difficult to disperse, is easy to reunite；It is excessive that then not enough, adsorption effect is poor for expansion surface product when heated.
After the completion of S30, premix, brominated polystyrene, antimony oxide are added according to the weight ratio, continues to use high mixer
It is mixed, until each component is uniformly mixed；In the step, bromide fire retardant uses brominated polystyrene, and brominated styrene is to pass through
Styrene is subjected to ethylene linkage protection first, then carries out bromination, then ethylene linkage is restored, synthesize brominated styrene, then again into
Row polymerization is completed.It prevents bromating agent while parental materials occur on the phenyl ring of polystyrene, can also occur on main chain
A small amount of free radical replaces, and can reduce the adverse effect to product colour and thermal stability.
Extruder is sent into S40, the raw material that step S30 is mixed, discharging, carries out fusion plastification, kneading mixing, and alkali-free is short
Cut fiber and be added through Weightlessness balance by side feed material, most afterwards through head extrusion, tie rod, cooling, pelletizing, drying, can be obtained low-density,
66 material of low smell bromine system flame-retardant reinforced nylon.In the step, extruder is double screw extruder, and the draw ratio of extruder is
44:1, extruder temperature are 280 DEG C, screw speed 500rpm.In the step, the diameter of glass fibre is 10-14 μm, length
For 3-4.5mm；Under the length and diameter, glass fibre can be made to be easier to be uniformly dispersed during coextrusion, reach product
To better intensity.
Embodiment 2
S10,49 parts of PA66 resins are dried into 80 DEG C of dehumidifying device 6h, controls moisture less than 0.2%；The step
Middle PA66 resin uses polyamide 66 resin, polyamide 66 resin heat resistance with higher and cost performance.Wherein, PA66 resin
Fusing point be 270 DEG C, relative viscosity 3.0；
S20, by dried PA66 resin, 0.4 part of primary antioxidant, 0.6 part of in-lubricant and 5 parts of expanded graphites according to weight
Amount proportion premixes 5min in high mixer high speed；In the step, the phosphorus content ﹥ 99.5% of expanded graphite, partial size is 14 μm；
After the completion of S30, premix, brominated polystyrene, antimony oxide are added according to the weight ratio, continues to use high mixer
It is mixed, until each component is uniformly mixed；In the step, bromide fire retardant uses brominated polystyrene.
Extruder is sent into S40, the raw material that step S30 is mixed, discharging, carries out fusion plastification, kneading mixing, and alkali-free is short
Cut fiber and be added through Weightlessness balance by side feed material, most afterwards through head extrusion, tie rod, cooling, pelletizing, drying, can be obtained low-density,
66 material of low smell bromine system flame-retardant reinforced nylon.In the step, extruder is double screw extruder, and the draw ratio of extruder is
44:1, extruder temperature are 280 DEG C, screw speed 500rpm.
Embodiment 3
S10,51 parts of PA66 resins are dried into 89 DEG C of dehumidifying device 4h, controls moisture less than 0.2%；The step
Middle PA66 resin uses polyamide 66 resin, polyamide 66 resin heat resistance with higher and cost performance.Wherein, PA66 resin
Fusing point be 260 DEG C, relative viscosity 2.0；
S20, by dried PA66 resin, 0.5 part of primary antioxidant, 0.5 especially lubricant and 3 parts of expanded graphites according to weight
Amount proportion premixes 2min in high mixer high speed；In the step, the phosphorus content ﹥ 99.5% of expanded graphite, partial size is 13 μm；
After the completion of S30, premix, bromide fire retardant, antimony oxide are added according to the weight ratio, it is equal to continue to use high mixer
It is mixed, until each component is uniformly mixed；In the step, bromide fire retardant uses brominated Polystyrene.
Extruder is sent into S40, the raw material that step S30 is mixed, discharging, carries out fusion plastification, kneading mixing, and alkali-free is short
Cut fiber and be added through Weightlessness balance by side feed material, most afterwards through head extrusion, tie rod, cooling, pelletizing, drying, can be obtained low-density,
66 material of low smell bromine system flame-retardant reinforced nylon.In the step, the draw ratio of extruder is 44:1, and extruder temperature is 220 DEG C,
Screw speed is 500rpm.
Comparative example 1
S10,54 parts of PA66 resins are dried into 89 DEG C of dehumidifying device 4h, controls moisture less than 0.2%；
S20, by dried PA66 resin, 0.5 part of primary antioxidant, 0.5, especially lubricant is mixed in height according to the weight ratio
Machine high speed premixes 2min；
After the completion of S30, premix, brominated polystyrene, antimony oxide are added according to the weight ratio, continues to use high mixer
It is mixed, until each component is uniformly mixed；
Extruder is sent into S40, the raw material that step S30 is mixed, discharging, carries out fusion plastification, kneading mixing, and alkali-free is short
It cuts fiber and is added through Weightlessness balance by side feed material, comparative example 1 most can be obtained through head extrusion, tie rod, cooling, pelletizing, drying afterwards
Nylon material.
Comparative example 2
S10,44 parts of PA66 resins are dried into 89 DEG C of dehumidifying device 4h, controls moisture less than 0.2%；
S20, by dried PA66 resin, 0.5 part of primary antioxidant, 0.5, especially lubricant is mixed in height according to the weight ratio
Machine high speed premixes 2min；
After the completion of S30, premix, brominated polystyrene agent, antimony oxide are added according to the weight ratio, continues to use high mixed
Machine is mixed, until each component is uniformly mixed；
Extruder is sent into S40, the raw material that step S30 is mixed, discharging, carries out fusion plastification, kneading mixing, and alkali-free is short
It cuts fiber and is added through Weightlessness balance by side feed material, it, can 2 nylon of comparative example most afterwards through head extrusion, tie rod, cooling, pelletizing, drying
Material.
For inspection low-density provided by the invention, the application of low smell bromine system flame-retardant reinforced nylon 66 in practice, carry out
Property test.And carried out according to Volkswagen interior trim smell test method PV3900, test judgment criteria is divided into 1-6 grades, while
The case where being likely to occur between two kinds of grades.Score 1 odorlessness；It scores 2 odorous, but non interference smell；Scoring 3 has
Obvious smell, but non interference smell；Scoring 4 has interference smell；Scoring 5 has strong interference smell；Scoring 6 has and cannot bear
By smell.It is as shown in table 2 to test structure:
Table 2
The oder levels of comparative example 1, embodiment 2, embodiment 3 and comparative example 1, it is known that, in the bromine system of close number
Under fire retardant, the oder levels in each embodiment are below comparative example 1.Comparative example 1, embodiment 2, embodiment 3 and comparison
The oder levels of example 2, it is known that, comparative example 2 need to add bromide fire retardant than 58%-75% more in embodiment can be only achieved with
The identical oder levels of each embodiment.It can be seen that nylon PA66 provided by the invention, can be effectively improved smell problem, and
And effectively reduce the dosage of bromide fire retardant.
The density of comparative example 2, embodiment 3 and comparative example 1, it is known that, under the bromide fire retardant of equal parts, implement
The density of example 2 and embodiment 3 is respectively less than comparative example 1, it can be seen that, nylon PA66 provided by the invention is being effectively improved smell
In the case where, greatly reduce the density of material, can satisfy lightweight requirements automobile, both mechanically and electrically electric appliance etc. lead
Domain.
Expanded graphite is typical layer structure, there is a fixed gap between layers, under heating condition, three oxidations two
Antimony element in antimony makes bromide fire retardant generate more bromine free radicals at a lower temperature, and bromine free radical enters the interlayer of graphite
Gap forms intercalation compound with carbon network plane, which meets pyrolytic, generate a kind of thrust, keep graphite linings high power swollen
Swollen, absorption smell forms the carbon-coating of height on the surface of the material simultaneously, plays starvation, heat-insulated effect, which is in antimony
Promote the synergistic effect of lower graphite and bromide fire retardant.Also fire-retardant, reduction density is therefore played, smell is reduced, improves glowing filament
The effect of initiation temperature.
The present invention greatly reduces the resistance of bromine system by the synergistic effect of expanded graphite and antimony oxide, bromide fire retardant
The dosage of agent is fired, and has reached excellent flame retardant effect, thereby also reduces the density of material, and generate expansion because graphite is heated
There is suction-operated, reduces the odor profiles of material.The glowing filament ignition temperature of material can also be improved simultaneously.
Preparation method provided by the invention keeps the moisture content of PA66 resin small by carrying out removal moisture drying to PA66 resin
In 0.2%.Avoid it is unseasoned, due to moisture it is excessively high and cause in process moisture easily make PA66 resin hydrolyzing, to drop
The problem of low material property.
Then it is premixed by high speed before production, enables PA66 resin together with processing aid, expanded graphite close adhesion,
It is not easy to disperse, each component can be distributed more uniform in subsequent extrusion process, and the material property of preparation is more stable.It avoids
Due to PA66 resin and processing aid, expanded graphite this three's work in-process poor dispersion, product is reduced caused by being unevenly distributed
Performance, such as strength problem.
It is prepared again by the extruder mirror image set with specific draw ratio, revolving speed and temperature；Wherein, extruder is specific
Draw ratio is to cause the melting effect of each component in an extruder poor in order to avoid draw ratio is too small；It is excessive that each component is caused to exist
Extruder extended residence time makes material lead to the problem of decomposition.Extruder specific rotation speeds and temperature setting are in order to avoid turning
The problem of speed and temperature are higher, and the shear heat of generation is excessively high, easily decompose material.
Preparation method provided by the invention has prepared low-density, low smell bromine system by the collaboration between each step
Flame-retardant reinforced nylon 66.
Although more herein used such as PA66 resin, bromide fire retardant, antimony oxide, expanded graphite, glass
The terms such as glass fiber, processing aid, but it does not exclude the possibility of using other terms.The use of these items is only for more
Easily describe and explain essence of the invention；Being construed as any additional limitation all is and spirit of that invention phase
It violates.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (8)
1. a kind of low-density, low smell bromine system flame-retardant reinforced nylon 66, it is characterised in that: the component matched by following parts by weight
It constitutes:
2. low-density, low smell bromine system flame-retardant reinforced nylon 66 according to claim 1, it is characterised in that: the PA66 tree
Rouge is adipic acid and the polyamide 66 resin that hexamethylene diamine polycondensation reaction obtains；The fusing point of the PA66 resin is 250-270 DEG C, phase
It is 2.0-3.0 to viscosity.
3. low-density, low smell bromine system flame-retardant reinforced nylon 66 according to claim 1, it is characterised in that: the bromine system resistance
Combustion agent is at least one of brominated polystyrene, brominated Polystyrene, decabromodiphenylethane.
4. low-density, low smell bromine system flame-retardant reinforced nylon 66 according to claim 1, it is characterised in that: the glass fibers
Dimension is alkali-free chopped strand；The diameter of the glass fibre is 10-14 μm, length 3-4.5mm.
5. low-density, low smell bromine system flame-retardant reinforced nylon 66 according to claim 1, it is characterised in that: the expansion stone
The phosphorus content ﹥ 99.5% of ink, partial size are 12-14 μm.
6. low-density, low smell bromine system flame-retardant reinforced nylon 66 according to claim 1, it is characterised in that: the processing helps
Agent is the combination of one or more of primary antioxidant, auxiliary anti-oxidant, in-lubricant and external lubricant.
7. the preparation method of a kind of low-density, low smell bromine system flame-retardant reinforced nylon 66, it is characterised in that: using such as claim
The described in any item low-density of 1-6, low smell bromine system flame-retardant reinforced nylon 66, the preparation method is specific as follows:
S10, PA66 resin is dried into 80-90 DEG C of dehumidifying device 4-6h, controls moisture less than 0.2%；
S20, dried PA66 resin, processing aid and expanded graphite are premixed into 2- in high mixer high speed according to the weight ratio
5min；
After the completion of S30, premix, bromide fire retardant, synergistic flame retardant are added according to the weight ratio, continues to use high mixer and mixes,
Until each component is uniformly mixed；
Extruder is sent into S40, the raw material that step S30 is mixed, discharging, carries out fusion plastification, kneading mixing, alkali-free is chopped fine
Dimension is added through Weightlessness balance by side feed material, and low-density, low gas most can be obtained through head extrusion, tie rod, cooling, pelletizing, drying afterwards
66 material of taste bromine system flame-retardant reinforced nylon.
8. low-density, the preparation method of low smell bromine system flame-retardant reinforced nylon 66 according to claim 7, it is characterised in that:
The draw ratio of extruder described in step S40 is 44:1, and extruder temperature is 220-280 DEG C, screw speed 300-600rpm.
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| CN111892813A (en) * | 2020-07-28 | 2020-11-06 | 横店集团得邦工程塑料有限公司 | Low-odor reinforced toughened flame-retardant PA6 composite material and preparation method thereof |
| CN113817314A (en) * | 2020-06-18 | 2021-12-21 | 中国石油化工股份有限公司 | Composition for flame-retardant floating cover, flame-retardant floating cover material and preparation method of flame-retardant floating cover material |
| CN113956654A (en) * | 2021-10-22 | 2022-01-21 | 安徽众诚塑胶科技有限公司 | High-temperature-resistant nylon master batch and preparation method thereof |
| CN114213838A (en) * | 2021-12-03 | 2022-03-22 | 上海金发科技发展有限公司 | Flame-retardant nylon composite material with low pungent smell and preparation method and application thereof |
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| CN114213838A (en) * | 2021-12-03 | 2022-03-22 | 上海金发科技发展有限公司 | Flame-retardant nylon composite material with low pungent smell and preparation method and application thereof |
| CN114213838B (en) * | 2021-12-03 | 2024-03-15 | 上海金发科技发展有限公司 | Flame-retardant nylon composite material with low pungent smell and preparation method and application thereof |
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