CN106832904A - A kind of halogen-free flame-retardant nylon material and its preparation method and application - Google Patents
A kind of halogen-free flame-retardant nylon material and its preparation method and application Download PDFInfo
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- CN106832904A CN106832904A CN201710101823.7A CN201710101823A CN106832904A CN 106832904 A CN106832904 A CN 106832904A CN 201710101823 A CN201710101823 A CN 201710101823A CN 106832904 A CN106832904 A CN 106832904A
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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
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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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
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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Abstract
The invention belongs to engineering plastic modification technical field, a kind of halogen-free flame-retardant nylon material and its preparation method and application is disclosed.Halogen-free flame-retardant nylon material of the invention presses weight/mass percentage composition includes following components：Nylon 6 20~80%；The copolymer 20~80% of nylon 6；Halogen-free flame retardants 1~8%；Heat stabilizer 0.1~1%；Processing aid 0.1~1%；The mass percent of said components amounts to 100%.Halogen-free flame-retardant nylon material of the invention using by hexamethylene diamine and carbon atom quantity 9~14 dicarboxylic acids polycondensation long-chain nylon, it has good compatibility with PA6, the material for obtaining has good pliability and lower temperature resistance, and do not influence the anti-flammability of triazines halogen-free flame retardants, with good heat aging property, good lower temperature resistance, be very suitable for manufacture extrusion bellows etc., particularly car engine the room in the hot environment such as industrial electric in wire harness corrugated pipe and helix tube etc..
Description
Technical field
The invention belongs to engineering plastic modification technical field, more particularly to a kind of halogen-free flame-retardant nylon material and its preparation side
Method and application.
Background technology
Plastic film capicitor is largely used to the fields such as automotive wire bundle, instrument and meter, electronic apparatus, industrial electric, distribution system.
Be presently used for manufacture extrusion corrugated pipe is mostly polyolefine material, such as polypropylene PP, polythene PE, ethene-vinyl acetate
Ester copolymer EVA etc..But not only fusing point is low for these polyolefine materials, poor heat resistance, and oxygen index (OI) is very low, anti-flammability
Difference.In order to improve the degree of safety of car engine room and industrial electric, requirement of the people to bellows material heat resistance and anti-flammability
Also more and more higher, these polyolefine materials obviously cannot meet requirement.In order to improve the anti-flammability of polyolefin, it is necessary to add a large amount of
Halogen-free flame retardants, this obviously can reduce the toughness and extrusion molding processability of material.
Polyvinylchloride is also commonly used for manufacturing bellows, and although PVC has good flame-retardance and toughness concurrently, but near
Nian Lai, people's research finds that the halogen compounds such as brominated and chlorine are polluted and harmful to environment, with related environmental protection
The progressively implementation of laws and regulations, PVC material will increasingly be restricted.
Nylon PA has good mechanical mechanics property, toughness, chemical resistance, wearability, heat resistance, electrical property etc. excellent
Combination property, is also widely used in manufacturing bellows.But the anti-flammability of nylon PA is unsatisfactory.
The PP/PA corrugated tube composite material of patent CN102050993A inventions, material is improved using bromide fire retardant
The anti-flammability of material, the human health but bromide fire retardant pollutes the environment and endangers.
Patent US3660344 and US5567797 use the compound in triazine class such as conduct such as melamine, melamine cyanurate
The halogen-free flame retardants of nylon, although these compound in triazine class can improve the anti-flammability of nylon material, but reduces nylon
The pliability of material.
Some polyolefin elastomers and nylon blending are added, the toughness of nylon material can be improved, but these polyolefin bullets
Gonosome can reduce the anti-flammability of nylon material, and the flame retarding efficiency of triazines halogen-free flame retardants can be especially greatly reduced.
Therefore, develop and have excellent toughness and anti-flammability, halogen free flame-retarded nylon 6 environmentally friendly, for extruding bellows concurrently
Imperial material, it appears particularly important.
The content of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, primary and foremost purpose of the invention is to provide a kind of halogen-free flameproof
Nylon material, it has good toughness and anti-flammability concurrently, while also having good heat aging property, resistance to low temperature.
Another object of the present invention is to provide a kind of preparation method of above-mentioned halogen-free flame-retardant nylon material.
Still a further object of the present invention is the application for providing above-mentioned halogen-free flame-retardant nylon material in manufacture extrusion bellows, special
Wire harness corrugated pipe and helix tube not being suitable in car engine room and in industrial electric etc..
The purpose of the present invention is realized by following proposal：
A kind of halogen-free flame-retardant nylon material, following components is included by weight/mass percentage composition：
The mass percent of said components amounts to 100%.
It is furthermore preferred that the halogen-free flame-retardant nylon material to press weight/mass percentage composition composed of the following components：
The mass percent of said components amounts to 100%.
Described nylon 6, is extrusion grade PA6, relative viscosity between 2.8~5.0, more preferably 3.0~4.5.
The described copolymer of nylon 6, is the copolymer of nylon 6 and long-chain nylon；
Wherein, long-chain nylon is formed by hexamethylene diamine and carbon atom quantity in 9~14 dicarboxylic acids polycondensation；
Dicarboxylic acid molecule formula is HOOC- (CH2) R-COOH, wherein R=7~12.
Described long-chain nylon is preferably at least one in PA69, PA610, PA611, PA612, PA613, PA614.
The described copolymer of nylon 6 is preferably PA6/69, PA6/610, PA6/611, PA6/612, PA6/PA613, PA6/
At least one in PA614 copolymers.
Had with PA6 in the long-chain nylon of 9~14 dicarboxylic acids polycondensation by hexamethylene diamine and carbon atom quantity good
Compatibility, is blended the copolymer nylon for preparing, and with good pliability and lower temperature resistance, and does not influence triazines halogen-free flame retardants
Anti-flammability.
Described halogen-free flame retardants is triazine based flame retardant, is preferably included in melamine and melamine cyanurate at least
It is a kind of.
Described heat stabilizer includes N, N'- is double-(3- (3,5- di-tert-butyl-hydroxy phenyls) propiono) hexamethylene diamine,
Four [β-(3,5- di-tert-butyl-hydroxy phenyls) propionic acid] pentaerythritol esters, three (2,4- di-tert-butyl-phenyls) phosphite esters, four
(2,4- di-tert-butylphenols) -4,4- xenyls diphosphites, double (2,6- di-t-butyl -4- aminomethyl phenyls) phosphorus of pentaerythrite two
In acid esters at least two.
Described processing aid includes N, and N'- ethylene bis stearamides, calcium stearate, zinc stearate, pentaerythrite are stearic
At least one in acid esters, silicone series lubricant agent and Tissuemat E.
The present invention also provides a kind of above-mentioned halogen-free flame-retardant nylon material preparation method, comprises the following steps：
Nylon resin, halogen-free flame retardants, heat stabilizer, processing aid are dried, is then well mixed and is added to twin-screw
In the hopper of extruder, through melt blending extrusion, cooling, air-dried, granulation, the halogen-free flame-retardant nylon material is obtained.
Wherein, double screw extruder processing temperature is 180~250 DEG C, 300~500 revs/min of screw speed.
The present invention also provides application of the above-mentioned halogen-free flame-retardant nylon material in manufacture extrusion bellows, is particularly suitable for vapour
Wire harness corrugated pipe and helix tube in car engine chamber and in industrial electric etc..
The tubing such as manufacture bellows, in order to reach preferable extrusion molding processability, general selection molecular weight is larger, melt
The less viscous nylon resin high of flow rate, i.e., it is general between 2.8~5.0 from nylon relative viscosity, relative viscosity 3.0~
It is more particularly suitable between 4.5.
Nylon corrugated tube and helix tube etc. can be protected in -40 DEG C to 120 DEG C temperature ranges, it is necessary to have good toughness
Hold good pliability.Tension fracture elongation rate is higher, and stretch modulus is smaller, then the pliability of material is better.Therefore, not only need
Wanting nylon material has tension fracture elongation rate higher, in addition it is also necessary to have relatively low stretch modulus.
In addition, during nylon corrugated tube extrusion, extrusion temperature scope is general between 190~260 DEG C；Nylon
The preferable scope of fusing point is between 180~250 DEG C.Fusing point is too high, then extrusion temperature is higher, and halogen-free flame retardants can be produced point
Solution；And fusing point is too low, then in extrusion, the heat resistance of nylon material can deteriorate decline.
Meanwhile, nylon corrugated tube need to have good anti-flammability, i.e. oxygen index (OI) to be not less than 23.When the oxygen index (OI) of material is not small
When 22, with self-extinguishment, after leaving burning things which may cause a fire disaster, will not continuous burning in atmosphere.Although after nylon water suction, oxygen index (OI) can reach
23, but in dry state, oxygen index (OI) is less than 23.
Halogen-free flame-retardant nylon material of the invention, by adjusting each component ratio, is obtained and has excellent toughness and anti-flammability concurrently
Environmentally friendly nylon material, while also have good heat aging property and lower temperature resistance；It is very suitable for extruding ripple
Wire harness corrugated pipe and helix tube in line tubing, such as car engine room and in industrial electric.
The present invention has the following advantages and beneficial effect relative to prior art：
Fire-retardant nylon material of the invention is free from the environmentally friendly material of halogen, has good toughness and fire-retardant concurrently
Property；Also there is good heat aging property, good lower temperature resistance simultaneously.
Halogen-free flame-retardant nylon material of the invention is very suitable for manufacture extrusion bellows etc., such as in car engine room and work
Industry wire harness corrugated pipe and helix tube electrically etc. in hot environment etc..
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
Following components is used in the embodiment of the present invention and comparative example：
Nylon 6 is extrusion grade PA6, relative viscosity：3.4, fusing point：225 DEG C, using purchased from the beautiful CM1021FS in east.
The copolymer of nylon 6 is the copolymer of nylon 6/610 (mass parts of 6 accounting of nylon 50%, the mass of NYLON610 accounting 50%
Part), relative viscosity：3.6, fusing point：145℃.
The copolymer of nylon 6/610 can be prepared via a method which to obtain：
80kg caprolactams and 2500mL water are put into the autoclave of 400L, nitrogen are filled with and are excluded oxygen and closed.
Reactor is warming up to 150 DEG C, and then by 200kg, the hexamethylene sebacamide aqueous solution of 40% mass concentration is added by measuring pump
In reactor, at 150 DEG C, internal pressure 2.5kg, unlatching is slowly stirred reactor temperature.It is to be mixed it is uniform after, in reactor
Temperature rises to 260 DEG C, and internal pressure rises to 10kg；When temperature rises to 260 DEG C, reacting kettle inner pressure is slowly reduced, reacted
Mixture in the kettle mixed melting under the conditions of appropriate power of agitator reacts.After 2h, nitrogen is filled with, makes to be protected in reactor
Atmospheric pressure state is stayed, stops stirring.Products therefrom extrusion, Cast Strip, pelletizing.Further by extracting in boiling water, unreacted list is eliminated
Body.Then dry, both obtain PA6/610 copolymers.
Halogen-free flame retardants is melamine cyanurate MCA, using purchased from Hangzhou JLS Flame Retardants Chemical Co., Ltd.
MC-25。
Heat stabilizer is N, N'- couples-(3- (3,5- di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine, the trade mark
IRGANOX 1098, purchased from BASF.
Heat stabilizer is double (2,6- di-t-butyl -4- aminomethyl phenyls) pentaerythritol diphosphates, and trade mark PEP-36 is purchased from
Adeka。
Processing aid is calcium stearate, purchased from Zhongshan Huamingtai Chemical Co., Ltd..
The specific preparation method of embodiment and comparative example is comprised the following steps：
Content weighs raw material by mass percentage；Nylon resin, halogen-free flame retardants, heat stabilizer, processing aid are dried,
Then it is well mixed and is added in the hopper of double screw extruder, through melt blending extrusion, cooling, air-dried, granulation, is obtained described
Halogen-free flame-retardant nylon material；Wherein, a diameter of 35mm of double-screw extruder screw, draw ratio is 36:1, double screw extruder adds
Work temperature is 200~230 DEG C, 350~450 revs/min of screw speed.
In following embodiment and comparative example, material property tests assessment by the following method.
Relative viscosity：Testing standard is ISO 307-2007；
Fusing point：Melting peak temperature is tested by DSC (differential scanning calorimeter), melting temperature value is obtained final product；
Stretch modulus：Assessment rigidity, testing standard is ASTM D638；
Tension fracture elongation rate：Assessment toughness, testing standard is ASTM D638, and batten size is thickness 1mm, area
200mm2；23 DEG C of test condition air humidity 55%, room temperature；
Oxygen index (OI)：Assessment anti-flammability, testing standard is ASTM D2863, and oxygen index (OI) tests (moisture content in nylon dry state
≤ 0.3%)；
Heat-proof aging is tested：Batten is placed in thermal aging oven, 130 DEG C/500 hours；Then take out batten wet in air
After being placed 48 hours at degree 55%, 23 DEG C of room temperature, tension fracture elongation rate is tested；
Low temperature resistant test：Under the conditions of -40 DEG C (- 40 DEG C of batten pre-treatment, 8 hours), tension fracture elongation rate is tested.
The constituent (based on weight/mass percentage composition) and test result of comparative example and embodiment are as shown in Table 1 and Table 2.
The halogen-free flame-retardant nylon material constituent mass percentage composition of table 1 and the performance test results
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | |
| Nylon 6 | 97.2 | 95.2 | 89.2 | 27.2 | 38.2 |
| The copolymer of nylon 6/610 | 0 | 0 | 0 | 70 | 60 |
| MCA fire retardants | 2 | 4 | 10 | 2 | 1 |
| Heat stabilizer 1098 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
| Heat stabilizer PEP-36 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
| Calcium stearate | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Oxygen index (OI) (%) | 24.2 | 27.0 | 33.5 | 23.5 | 22.3 |
| Fusing point (DEG C) | 225.0 | 225.0 | 225.0 | 167.8 | 182.6 |
| Stretch modulus (MPa) | 980 | 1000 | 1080 | 250 | 270 |
| Elongation at break (%) | 68.4 | 48.3 | 18.0 | 192.5 | 188.0 |
| Elongation at break (%) after heat ageing | 28.3 | 22.6 | 8.8 | 90.2 | 86.4 |
| - 40 DEG C of freezing crack elongations (%) | 16.8 | 11.2 | 3.7 | 60.6 | 57.3 |
The halogen-free flame-retardant nylon material constituent mass percentage composition of table 2 and the performance test results
According to Tables 1 and 2 experimental result data：
Embodiment 1 is blended, no using PA6 and PA6/610 copolymers to the nylon material of embodiment 6 in suitable ratio
Halogen-containing flame retardant, with good anti-flammability and melting temperature higher；Simultaneously there is good toughness, by 130 DEG C/
After 500h heat ageings and -40 DEG C of low-temperature tests, still retain elongation at break higher.
The nylon material of comparative example 1,2,3, is used alone PA6, and stretch modulus is too high, and elongation at break is too low, and rigidity is partially
Height, toughness is too poor.The nylon material fusing point of comparative example 4 is too low, and heat resistance is not enough.The nylon material oxygen index (OI) of comparative example 5 is relatively low,
Anti-flammability is unsatisfactory.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of halogen-free flame-retardant nylon material, it is characterised in that include following components by weight/mass percentage composition：
2. halogen-free flame-retardant nylon material according to claim 1, it is characterised in that by weight/mass percentage composition by following components
Composition：
3. halogen-free flame-retardant nylon material according to claim 1, it is characterised in that：Described nylon 6, is extrusion grade PA6,
Relative viscosity is between 2.8~5.0.
4. halogen-free flame-retardant nylon material according to claim 1, it is characterised in that：The described copolymer of nylon 6, is nylon
6 and the copolymer of long-chain nylon；Wherein, long-chain nylon is formed by hexamethylene diamine and carbon atom quantity in 9~14 dicarboxylic acids polycondensation；
Dicarboxylic acid molecule formula is HOOC- (CH2) R-COOH, wherein R=7~12.
5. halogen-free flame-retardant nylon material according to claim 4, it is characterised in that：Described long-chain nylon be PA69,
At least one in PA610, PA611, PA612, PA613 and PA614.
6. halogen-free flame-retardant nylon material according to claim 1, it is characterised in that：The described copolymer of nylon 6 is PA6/
69th, at least one in PA6/610, PA6/611, PA6/612, PA6/PA613 and PA6/PA614 copolymer.
7. halogen-free flame-retardant nylon material according to claim 1, it is characterised in that：Described halogen-free flame retardants be include it is close
At least one in amine and melamine cyanurate.
8. halogen-free flame-retardant nylon material according to claim 1, it is characterised in that：Described heat stabilizer includes N, N'-
Double-(3- (3,5- di-tert-butyl-hydroxy phenyls) propiono) hexamethylene diamine, four [β-(3,5- di-tert-butyl-hydroxy phenyls) third
Acid] pentaerythritol ester, three (2,4- di-tert-butyl-phenyls) phosphite esters, four (2,4- di-tert-butylphenols) -4,4- xenyls two be sub-
In phosphate, double (2,6- di-t-butyl -4- aminomethyl phenyls) pentaerythritol diphosphates at least two；Described processing aid
Including N, N'- ethylene bis stearamides, calcium stearate, zinc stearate, pentaerythritol stearate, silicone series lubricant agent and poly- second
At least one in alkene wax.
9. the preparation method of the halogen-free flame-retardant nylon material described in a kind of any one of claim 1~8, it is characterised in that including with
Lower step：
Nylon resin, halogen-free flame retardants, heat stabilizer, processing aid are dried, is then well mixed and is added to twin-screw extrusion
In the hopper of machine, through melt blending extrusion, cooling, air-dried, granulation, the halogen-free flame-retardant nylon material is obtained；
Wherein, double screw extruder processing temperature is 180~250 DEG C, 300~500 revs/min of screw speed.
10. application of the halogen-free flame-retardant nylon material described in any one of claim 1~8 in manufacture extrusion bellows.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115490921A (en) * | 2022-08-18 | 2022-12-20 | 浙江万盛股份有限公司 | High-efficiency phosphite ester solid antioxidant composition and nylon 66 synthetic resin composition using same |
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Application publication date: 20170613 |