CN109735103A - It soaks resistance to precipitation flame retardant polyamide composite material and preparation method thereof - Google Patents
It soaks resistance to precipitation flame retardant polyamide composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of resistance to precipitation flame retardant polyamide composite materials of immersion and preparation method thereof, it soaks resistance to precipitation flame retardant polyamide composite material, by 65-90 part polyamide, 8-25 parts of silica modified melamine cyanurates, the 0.5-5 parts of epoxy polysiloxanes, 0.5-5 parts of following parts by weight；0.1-1 parts of antioxidant, 0.1-1 parts of lubricants soak resistance to precipitation flame retardant polyamide composite material to obtain the final product by double-screw extruding pelletizing.The halogen-free flame-retardant polyamide material of the resistance to precipitation of immersion prepared by the present invention has many advantages, such as flame retarding efficiency height, good toughness, the resistance to precipitation of immersion and simple processing, is widely used in electronic and electrical field.
Description
Technical field
The present invention relates to polyamide compoiste material technical fields, and in particular to a kind of immersion halogen-free flame-retardant polyamide of resistance to precipitation
Composite material and preparation method.
Background technique
Polyamide is as engineering plastics, mechanical performance with higher, impact property, and higher heat resistance is good resistance to
Chemical property and it is easily molded the features such as, be widely used in the fields such as automobile, electronic apparatus.However, polyamide produces in combustion
Raw molten drop phenomenon, generation largely have flame molten drop, are easy to cause second-time burning.So being needed in the use process of polyamide pair
Its progress is flame-retardant modified.
Currently, the flame-retardant system of polyamide is mainly bromine sb system, nitrogen system, phosphorus nitrogen system and inorganic mineral filling.Bromine antimony
Composite flame-proof polyamide has excellent flame retardant property, while keeping good processing performance and mechanical performance, but bromine antimony hinders
It fires agent and generates volume of smoke and corrosivity pernicious gas in burning, which uses and received limitation.Phosphorus nitrogen body
It is that halogen-free flame retardants can compare favourably with traditional bromine antimony fire retardant, but phosphorus nitrogen systems price is high, can not promote the use of a large area.
A kind of halogen-free flame retardants of the melamine cyanurate (MCA) as high nitrogen-containing has high decomposition temperature, low
Cigarette, it is nontoxic and cheap the advantages that, have become halogen-free flame retardants application in preferred halogen-free flame retardants.But MCA makees
Poor with polyamide-compatible for filled-type fire retardant, the mechanical property of materials is greatly lowered after addition fire retardant and material is long
Fire retardant is easy to migrate to material surface after time places, and causes product surface frosting.It is fire-retardant especially under high temperature and humidity effect
Agent precipitation rate is accelerated, the final service performance for influencing product.
Publication No. CN 103897128A (application No. is 201410158223.0) Chinese patent application discloses a kind of resistance
Agent aggretion type MCA compound and preparation method thereof is fired, graft modification is carried out to melamine, then react generation with cyanuric acid
Salt.Aggretion type MCA reduces the precipitation rate of fire retardant since flame retardant molecule amount increases to a certain extent.
Summary of the invention
It is an object of the invention to solve defect existing for above-mentioned MCA Flameproof polyamide technology of preparing, a kind of leaching is provided
The flame retardant polyamide composite material and preparation method thereof of the resistance to precipitation of water.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of resistance to precipitation flame retardant polyamide composite material of immersion, is made of the material of following parts by weight:
The polyamide is one or both of PA6, PA66.
The innovation of the invention consists in that introducing silica on the surface fire retardant MCA, fire retardant is limited by silica
The migration of MCA (melamine cyanurate), while the inorganic silicon components of porous structure are introduced, improve material block heat resistance
Can, it reduces molten drop in polyamide combustion process and generates, improve the flame retardant property of material.Also, made using epoxy polysiloxane
The compatibility that fire retardant (silica modified melamine cyanurate) and polyamide are promoted for epoxy polysiloxane, into
The migration of one step reduction fire retardant.Meanwhile passing through epoxy group and fire retardant (silica modified melamine cyanurate)
Surface amino groups reaction improves material in fire retardant (silica modified melamine cyanurate) surface enrichment siloxane layer
Toughness, so that compensating for toughness caused by fire retardant adds reduces.The material has excellent mechanical performance, while material is in height
It is non-blooming for a long time under warm high humidity environment, it is suitable for delicate electrical circuit field.
Further preferably, the resistance to precipitation flame retardant polyamide composite material of the immersion, by the material of following parts by weight
Composition:
Still more preferably, the resistance to precipitation flame retardant polyamide composite material of the immersion, by the material of following parts by weight
Material composition:
The preparation of the silica modified melamine cyanurate includes:
(1) cetyl trimethylammonium bromide is dissolved in the mixed liquor of ether and ethyl alcohol, adds melamine isocyanic acid
After ester, ammonia spirit is then added in ultrasonic disperse, and mechanical stirring obtains mixture；
(2) it is stirred after ethyl orthosilicate being added in the mixture that step (1) obtains, three second of γ-aminopropyl is then added
Continue to stir after oxysilane, obtain white solid, more empty silica packets are dried to obtain after filtering, washing, ethyl alcohol are washed
Cover melamine cyanurate.
In step (1), the cetyl trimethylammonium bromide, ether, ethyl alcohol, melamine isocyanates, ammonium hydroxide
The amount ratio of solution is 50g:1000mL~3000mL:2000mL~4000mL:400g~600g:4000g~6000g, into one
Step is preferably 50g:1500mL~2500mL:2500mL~3500mL:450g~550g:4500g~5500g, further preferably
For 50g:2000mL:3000mL:500g:5000g.
Ultrasonic disperse 5-15min,
The pH of the ammonia spirit is 9-10.
The churned mechanically condition are as follows: mechanical stirring 0.2h~1h at 20 DEG C~30 DEG C；Further preferably, in 25
Mechanical stirring 0.5h at DEG C.
Cetyl in step (2), in the ethyl orthosilicate, gamma-aminopropyl-triethoxy-silane and step (1)
The ratio between trimethylammonium bromide dosage is 200g~300g:30g~70g:30g~70g, further preferably 240g~260g:40g
~60g:40g~60g, most preferably 250g:50g:50g.
2h~6h is stirred after ethyl orthosilicate is added, further preferably, stirs 3h~5h after ethyl orthosilicate is added, it is optimal
Choosing stirs 4h after ethyl orthosilicate is added.
Continue to stir 2h~6h after gamma-aminopropyl-triethoxy-silane is added, further preferably, γ-aminopropyl three is added
Continue to stir 3h~5h after Ethoxysilane, most preferably, continues to stir 4h after gamma-aminopropyl-triethoxy-silane is added.
The condition of the drying are as follows: dry 18h~30h at 70 DEG C~90 DEG C, further preferably, at 75 DEG C~85 DEG C
Lower dry 22h~26h is most preferably dried for 24 hours at 80 DEG C
The epoxy polysiloxane is terminal epoxy polysiloxanes and side group epoxy polysiloxanes compound, and terminal epoxy is poly-
Siloxanes and side group epoxy polysiloxanes weight ratio are 3:1-1:1, viscosity of polysiloxane 500-2000mm2/ s, epoxide number are
0.6-0.9。
The antioxidant is one or both of 1098,168.
The lubricant is ethylene bis stearic acid amide, modified ethylene bis-fatty acid amides (TAF), stearate, gathers
One of ethylene waxes are two or more (including two kinds).
The resistance to preparation method that flame retardant polyamide composite material is precipitated of the immersion, comprising the following steps:
By polyamide, silica modified melamine cyanurate, epoxy polysiloxane, antioxidant, lubricant by double
The charging of Screw Extrusion owner's spout, it is tie rod, cold after the abundant fusion plastification of material by under twin-screw conveying and shear action
But, pelletizing obtains the resistance to precipitation halogen-free fire-retarding reinforced polyamide composite material that soaks.
The temperature of fusion plastification is 220 DEG C -265 DEG C in the double screw extruder, and screw rod revolution is 400rpm/min
~600rpm/min.
Compared with prior art, the present invention has the advantage that
(1) modified to MCA fire retardant surface to introduce porous silica protective layer, protection and barrier action are played to MCA,
Reduce migration of the MCA fire retardant under high temperature and humidity effect；
(2) MCA flame-retardant system introduces organosilicon composition, by nitrogen-silicon flame retardant synergism, promotes material flame retarding efficiency,
Reach material combustion and do not generate molten drop, meets UL94V-0 requirement；
(3) siloxanes long-chain is introduced by chemical reaction in extrusion process on fire retardant rigid particles surface, is promoted fire-retardant
The compatibility of agent and polyamide, while improving the toughness of material.
(4) the halogen-free flame-retardant polyamide material of the resistance to precipitation of immersion prepared by the present invention has flame retarding efficiency height, good toughness, leaching
The advantages that resistance to precipitation of water and simple processing, it is widely used in electronic and electrical field.
Specific embodiment
Below with reference to embodiment, the invention will be further described:
Polyamide 66 (Hua Feng, 1106), polyamide 6 (newly drawing, 2500), lubricant TAF (Xingtai state light), silica change
Property melamine cyanurate (self-control), epoxy polysiloxane (DOW CORNING, DC345), melamine cyanurate (BASF),
1098 (commercially available).
Examples 1 to 3 and comparative example 1~2
The preparation of silica modified melamine cyanurate includes:
(1) 50g cetyl trimethylammonium bromide is dissolved in 2000mL ether and 3000mL ethyl alcohol, adds 500g trimerization
Cyanamide isocyanates is placed in ultrasonic disperse 10min.The ammonia spirit that 5000g pH is 9.5, machinery at 25 DEG C of room temperature is then added
0.5h is stirred, mixture is obtained.
(2) 4h is stirred after 250g ethyl orthosilicate being added in said mixture, is then slowly added to 50g γ-aminopropyl
Triethoxysilane continues to stir 4h, and obtained white solid is dried for 24 hours at 80 DEG C after filtering, washing, ethyl alcohol are washed
After obtain silica modified melamine cyanurate.
Silica modified melamine cyanurate
By polyamide 66, polyamide 6, silica modified melamine cyanurate, epoxy polysiloxane and antioxidant
1098, lubricant TAF is fed by twin-screw extrusion owner's spout, by under twin-screw conveying and shear action, material is abundant
After fusion plastification, tie rod, cooling, pelletizing obtain resistance to precipitation flame retardant polyamide composite material of soaking, and the twin-screw squeezes
The temperature of fusion plastification is 235 DEG C -255 DEG C in machine out, and screw rod revolution is 500rpm/min.
Embodiment 1-3 and comparative example 1-2 material mixture ratio are specifically shown in Table 1.
Table 1
| Raw material | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 |
| PA66 | 45 | 45 | 45 | 45 | 45 |
| PA6 | 40 | 41 | 42 | 40 | 40 |
| Silica modified MCA | 14 | 13 | 12 | / | 14 |
| MCA | / | / | / | 14 | / |
| Antioxidant 1098 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
| Epoxy polysiloxane | 1 | 1.5 | 2 | 0 | 0 |
| TAF | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
Gained pellet is molded into corresponding batten according to ISO testing standard, then in 23 ± 2 DEG C, 50 ± 5% relative humidity
It places under environment and is tested afterwards for 24 hours.The resistance to precipitation test of fire retardant is measured fire retardant in water afterwards for 24 hours by material boiling water treating and contained
Amount, tests that the results are shown in Table 2.
Table 2
| Project | Unit | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 |
| Tensile strength | MPa | 65 | 62 | 60 | 60 | 66 |
| Bending strength | MPa | 115 | 113 | 110 | 104 | 119 |
| The impact of Charpy non-notch | kJ/m2 | 98 | 100 | 105 | 50 | 70 |
| Vertical combustion UL94 | Class | V-0 | V-0 | V-0 | V-2 | V-0 |
| Flame retardant agent content | ppm | 150 | 150 | 150 | 1000 | 250 |
Polyamide material obtained by embodiment 1-3 has excellent flame retardant property and toughness, and fire retardant migration rate is low, is applicable in
In fields such as precise electronic material, weaving electric appliances.
Comparative example 1~2
Comparative example 1 does not use modified MC A and epoxy polysiloxane, and comparative example 2 does not use epoxy polysiloxane.
Examples 1 to 3 is compounded using modified MC A with epoxy polysiloxane, and the flame retarding efficiency of system is increased substantially, fire-retardant
The toughness that material is maintained while performance gets a promotion is applicable to sophisticated electronic circuitry field.Silica modified melamine
Amine cyanurate introduces silica on the surface fire retardant MCA, limits fire retardant MCA (melamine cyanurea by silica
Hydrochlorate) migration, while introducing the inorganic silicon components of porous structure, improve material block heat resistance, reduce polyamide combustion
Molten drop generates during burning, improves the flame retardant property of material.
It above are only specific embodiments of the present invention, but the design concept of the present invention is not limited to this, it is all to utilize this structure
Think of makes a non-material change to the present invention, and should all belong to behavior that violates the scope of protection of the present invention.
Claims (10)
1. a kind of resistance to precipitation flame retardant polyamide composite material of immersion, which is characterized in that be made of the material of following parts by weight:
The polyamide is one or both of PA6, PA66.
2. the resistance to precipitation flame retardant polyamide composite material of immersion according to claim 1, which is characterized in that by following heavy
Measure the material composition of part:
3. the resistance to precipitation flame retardant polyamide composite material of immersion according to claim 1, which is characterized in that by following heavy
Measure the material composition of part:
4. the resistance to preparation method that flame retardant polyamide composite material is precipitated of immersion according to claim 1,2 or 3, special
Sign is, comprising the following steps:
By polyamide, silica modified melamine cyanurate, epoxy polysiloxane, antioxidant, lubricant by twin-screw
The charging of owner's spout is squeezed out, by under twin-screw conveying and shear action, after the abundant fusion plastification of material, tie rod, is cut at cooling
Grain obtains resistance to precipitation flame retardant polyamide composite material of soaking；
The polyamide is one or both of PA6, PA66.
5. the preparation method according to claim 4, which is characterized in that the silica modified melamine cyanurate
Preparation include:
(1) cetyl trimethylammonium bromide is dissolved in the mixed liquor of ether and ethyl alcohol, addition melamine isocyanates it
Afterwards, ultrasonic disperse, is then added ammonia spirit, and mechanical stirring obtains mixture；
(2) it is stirred after ethyl orthosilicate being added in the mixture that step (1) obtains, gamma-aminopropyl-triethoxy is then added
Continue to stir after silane, obtain white solid, is dried to obtain silica modified melamine after filtering, washing, ethyl alcohol are washed
Amine cyanurate.
6. preparation method according to claim 7, which is characterized in that in step (1), the cetyl trimethyl bromine
Change ammonium, ether, ethyl alcohol, melamine isocyanates, ammonia spirit amount ratio be 50g:1000mL~3000mL:2000mL~
4000mL:400g~600g:4000g~6000g.
7. preparation method according to claim 7, which is characterized in that in step (1), ultrasonic disperse 5-15min；
The pH of the ammonia spirit is 9-10；
The churned mechanically condition are as follows: mechanical stirring 0.2h~1h at 20 DEG C~30 DEG C.
8. preparation method according to claim 7, which is characterized in that in step (2), the ethyl orthosilicate, γ-ammonia
The ratio between cetyl trimethylammonium bromide dosage in propyl-triethoxysilicane and step (1) for 200g~300g:30g~
70g:30g~70g.
9. preparation method according to claim 7, which is characterized in that in step (2), stir 2h after ethyl orthosilicate is added
~6h；
Continue to stir 2h~6h after gamma-aminopropyl-triethoxy-silane is added；
The condition of the drying are as follows: dry 18h~30h at 70 DEG C~90 DEG C.
10. preparation method according to claim 7, which is characterized in that fusion plastification in the double screw extruder
Temperature is 220 DEG C -265 DEG C, and screw rod revolution is 400rpm/min~600rpm/min.
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| CN112980183A (en) * | 2019-12-18 | 2021-06-18 | 南京聚隆科技股份有限公司 | Precipitation-resistant halogen-free flame-retardant reinforced nylon material and preparation method thereof |
| CN114395124A (en) * | 2022-02-17 | 2022-04-26 | 江西中塑新材料科技有限公司 | Polyamide composite material and synthetic method thereof |
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