CN106700527A - Flame-retardant polyamide resin composition and preparation method thereof - Google Patents
Flame-retardant polyamide resin composition and preparation method thereof Download PDFInfo
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34922—Melamine; Derivatives thereof
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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
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/45—Heterocyclic compounds having sulfur in the ring
- C08K5/46—Heterocyclic compounds having sulfur in the ring with oxygen or nitrogen in the ring
- C08K5/47—Thiazoles
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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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Abstract
The invention relates to flame-retardant polyamide resin composition and a preparation method thereof. The prepared flame-retardant polyamide resin composition is prepared from 72.0wt%-95.0wt% of polyamide resin, 4.0wt%-20.0wt% of a melamine or melamine derivative, 1.0wt%-7.0wt% of a flame-retardant synergist and 0-1.0wt% of a processing aid. The preparation method of the flame-retardant polyamide resin composition comprises steps as follows: four substances including polyamide resin, the melamine or melamine derivative, the flame-retardant synergist and the processing aid are uniformly mixed, and the flame-retardant polyamide resin composition is obtained after cooling. Compared with traditional melamine urate flame-retardant polyamide, the flame-retardant polyamide resin composition has excellent glow wire resistance and flame-retardant efficiency.
Description
Technical field
The invention belongs to flame resistant polyamide resin field, and in particular to a kind of flame resistant polyamide resin composition and its preparation
Method.
Background technology
Polyamide is commonly called as nylon (PA), refers to the linear macromolecule containing recurring amide radical group on molecular backbone, when the year before last
Yield 3 × 106More than ton, it is that a kind of yield is big, wide in variety, purposes is wide, the general engineering plastic of high comprehensive performance, is also one
Plant important composite fibre materials.It is different according to carbon atom quantity purpose in polyamide units chain link, can be divided into PA6, PA11,
PA12, PA46, PA66, PA610, PA612, PAl010, heat resistant polyamide, Long Carbon Chain Polyamide and new polyamide bullet
The type such as gonosome and copolymer nylon.It is maximum with the yield of PA6, PA66 and consumption in polyamide series of products, account for gathering
The 90% of acid amides yield.
The fire-retardant approach of current polyamide has three kinds：
(1) fire retardant is added during PA engineering plastics melt modifications, fire retardant is dispersed in PA, not with engineering plastics
React, reach fire-retardant purpose.
(2) adding the fire-retardant molecule with reactive functionality, the molecule can react with PA, be grafted on PA macromolecular chains,
Reach fire-retardant purpose.
(3) flame-retardant monomer is introduced in the preparation process of PA, while PA polymer generating process between flame-retardant monomer
React generation fire retardant, reaches fire-retardant purpose.
Because melamine based flame retardant is similar to the chemical property of PA, the melamine-based flame retardant in the fire-retardant application of PA
Agent is more superior than the flame retardant effect of halogen containing flame-retardant and red phosphorus, and melamine based flame retardant in itself and catabolite low toxicity
Property, cater to the trend that current fire retardant develops to high-efficiency low-toxicity direction.But melamine based flame retardant and macromolecular material base
Compatability is poor, disperses uneven in the base, has a strong impact on the mechanical property of material.Melamine cyanurate (MCA) has
Have the advantages that efficient, Halogen, low toxicity, low cigarette and macromolecular material matrix compatibility are good, in the fire-retardant side of nylon-type macromolecular material
Face has obtained extensive use.But MCA fusing points are high, poor dispersion, neat coal amout is relatively low, layer of charcoal is loose, can not be formed densification guarantor
Sheath, reduces the flame retarding efficiency of MCA and the mechanical property of fire proofing.Due to the mechanical property to PA engineering plastics, fire-retardant
The all requirements more and more higher such as performance, dielectric properties, outward appearance, single fire retardant is often difficult to realize its corresponding index, resistance
Combustion agent compounding can strengthen the flame retardant effect and combination property of PA.Therefore, three development sides of current melamine based flame retardant
Xiang Shi：Exploitation novel melamine fire retardant, is modified to melamine cyanurate, and exploitation novel melamine base is fire-retardant
Agent compounding flame retardant.
Horrocks(Horrocks A R,Smart G,Kandola B,et al.Zinc stannate
interactions with flame retardants in polyamides.Part I:Synergies with
organobromine-containing flame retardants in polyamides 6(PA6)and 6.6(PA6.6)
[J].Polymer Degradation and Stability,2012,97(12):2503-2510.) have studied zinc stannate and three
Poly cyanamid based flameproofing compounds the synergy to PA6, and research finds：Melamine phosphate, 5% aryl of addition 10%
Phosphate and 7.5% zinc stannate flame-proof PA 6, LOI values are reached 26.5%, are tested by UL 94V-2；Additionally, zinc stannate only has
Compounded simultaneously with both phosphate and just show to act synergistically, but fire-retardant nylon flame retardant rating prepared by the method can only reach
To UL94V2 grades.
Lei Song and Yuan Hu (Ge H, Tang G, Hu W Z, et al.Aluminum hypophosphite
microencapsulated to improve its safety and application to flame retardant
polyamide 6[J].Journal of Hazardous Materials,2015,294:186-194.) using MCA to secondary phosphorus
Sour aluminium carries out microencapsulation, is made microcapsules hypo-aluminum orthophosphate (MCAHP) Flameproof polyamide.It is fire-retardant when MCAHP additions are 20%
The oxygen index (OI) of polyamide reaches 27.5%.But the oxygen index (OI) of the fire-retardant nylon prepared by the method improves unobvious.
Chinese invention patent application number 201610450042.4 report it is a kind of using phosphorus flame retardant, bromide fire retardant and
The method of metal oxide compounding prepares Flameproof polyamide, but the method preparation is the Flameproof polyamide containing halogen, it is impossible to
Cater to the environmental requirement of flame retardant non-halogen.Chinese Patent Application No. 2014107678896 is disclosed to be made using trithiocyanuric acid
For modifying agent is prepared for a kind of modified melamine cyanurate fire retardant, the invention Special attention will be given to trithiocyanuric acid and cyanogen urine
Acid is synthesized a kind of modified melamine cyanurate fire retardant of new structure, and sulphur and triazine with melamine simultaneously
Ring cooperative flame retardant effect, but fire retardant of the invention be improve fire-retardant nylon limited oxygen index and vertical combustion it is fire-retardant
Grade.Further accordance with document 1 (synthesis of melamine based flame retardant and its application study of fire-retardant Nylon 6, author：Wang Ningping, east
Hua Da (Master's thesis), in January, 2016) report trithiocyanuric acid modified melamine cyanurate fire retardant nylon
6 glow-wire ignition temperature can reach 750 DEG C according to GB1040.3-2006 standard testings GWIT, but can not reach GWIT
850 DEG C and more than.Therefore, how to prepare and a kind of not only improved fire-retardant limited oxygen index and vertical combustion flame retardant rating but also improve
The fire retardant of GWIT temperature, is the current technical issues that need to address.
The content of the invention
The present invention be directed to the deficiencies in the prior art, there is provided a kind of environment friendly non-halogen element, glow wire resistant temperature are high, highly effective flame-retardant
Flame resistant polyamide resin composition and preparation method thereof, the present invention is using melamine and its derivative and sulfenamide
The method of compound fire retarding synergist compounding has prepared the flame resistant polyamide resin composition of function admirable.With traditional melamine
Amine cyanurate Flameproof polyamide is compared, and the limited oxygen index of flame-retardant polyamide composition of the invention, vertical combustion are fire-retardant etc.
Level and GWIT temperature are improved, with extraordinary using effect.
For achieving the above object, the present invention is adopted the following technical scheme that：
A kind of flame resistant polyamide resin composition, the component and content of the flame resistant polyamide resin composition is as follows：
The fire retarding synergist is one or more of sulfenamide compound；
Flame retardant rating reaches UL94V-0 to the flame resistant polyamide resin composition after tested；LOI value >=34.0%；According to
Nonflammable temperature >=850 DEG C of GB/T5169.13-2006 standard testings.
Because the molecular linkage form of sulfenamide compound is similar to polyamide, therefore both have good compatibility,
Physical property influence on Flameproof polyamide is small；Meanwhile, the presence of sulfenamide key can effectively facilitate polyamide degradation process
Crosslinking, such that it is able to promote into charcoal, reduce the release of incendivity volatile matter, improve flame retarding efficiency；In addition it is this into charcoal mistake
Journey is cooperateed with the mutual of gas phase fire retardation of melamine derivative, further increases flame retarding efficiency.
As preferred technical scheme：
Flame resistant polyamide resin composition as described above, the sulfenamide compound is N, N- diethyl -2- benzos
Thiazolesulfenamide, N- oxygen diethylene -2-[4-morpholinodithio sulfenamide, N, N- dicyclohexyls -2-[4-morpholinodithio sulfenamide, N-
The tert-butyl group -2-[4-morpholinodithio sulfenamide, N cyclohexyl 2 benzothiazole sulfenamide, N- t-octyls -2-[4-morpholinodithio time sulphur
Acid amides or N, N- diisopropyl -2-[4-morpholinodithio sulfenamide.
Flame resistant polyamide resin composition as described above, the nylon 6 (PA6) of the polyamide, nylon 11
(PA11), nylon 12 (PA12), nylon 46 (PA46), nylon66 fiber (PA66), NYLON610 (PA610), nylon 612 (PA612),
Nylon 1010 (PAl010), heat resistant polyamide, Long Carbon Chain Polyamide, new polyamide elastomer and copolymer nylon etc..
Flame resistant polyamide resin composition as described above, the melamine derivative be melamine cyanurate,
Melamine phosphate, melamine hypophosphite, melamine polyphosphate or melamine borate salt；
Flame resistant polyamide resin composition as described above, the processing aid is stearic acid, calcium stearate, stearic acid
Zinc, tristerin, ethylene stearic amide, erucyl amide or montanic acid sodium.
As above the preparation method of any described flame resistant polyamide resin composition, by polyamide, melamine or
Melamine derivative, four kinds of material melts of fire retarding synergist and processing aid are well mixed, and Flameproof polyamide is obtained after cooling
Resin combination.
The preparation method of flame resistant polyamide resin composition as described above, the temperature of the melting mixing is 150-290
℃；The mode of the cooling is that pure water or High Purity Nitrogen atmosphere are cooled down；Purity >=99.9% of nitrogen in the High Purity Nitrogen atmosphere.
Beneficial effect：
A kind of flame resistant polyamide resin composition of the invention is using melamine and its derivative and sulfenamide
Highly effective flame-retardant Amilan polyamide resin composition is prepared after compound compounding；
A kind of flame resistant polyamide resin composition of the invention has flame retarding efficiency high, and heat endurance is good, glow wire resistant temperature
Degree is high；
A kind of flame resistant polyamide resin composition of the invention, due to the presence of sulfenamide compound, can effectively facilitate
Nylon in burning condensed phase into charcoal, and charcoal can be effectively participated in into polymeric material fuel combustion process, in material surface
Fine and close protective layer is formed, its fire resistance is improve.
Specific embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
Bright rather than limitation the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, art technology
Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Fixed scope.
Embodiment 1
A kind of preparation method of flame resistant polyamide resin composition, by PA6, melamine, N, N- diisopropyl -2- benzos
Thiazolesulfenamide and stearic acid melting mixing are stirred, and flame resistant polyamide resin composition is obtained after cooling；Wherein melt
The temperature of mixing is 150 DEG C；The mode of cooling is pure water cooling；Each component hundred in obtained flame resistant polyamide resin composition
Divide ratio as follows：Polyamide is 72.0wt%；Melamine is 20.0wt%；N, N- diisopropyl -2-[4-morpholinodithio time sulphur
Acid amides is 7.0wt%；Stearic acid is 1.0wt%.
The performance parameter of obtained flame resistant polyamide resin composition is：Flame retardant rating reaches UL94V-0, LOI after tested
It is 34.0% to be worth, and is 850 DEG C according to the GWIT of GB/T5169.13-2006 standard testings.
Embodiment 2
A kind of preparation method of flame resistant polyamide resin composition, by PA11, melamine cyanurate, N- t-octyls-
2-[4-morpholinodithio sulfenamide melting mixing is stirred, and flame resistant polyamide resin composition is obtained after cooling；Wherein melt mixed
The temperature of conjunction is 290 DEG C；The mode of cooling is cooled down for High Purity Nitrogen atmosphere, and the purity of nitrogen is 99.9% in High Purity Nitrogen atmosphere；Resistance
Each component percentage is as follows in retardant polyamide resin composition：Polyamide is 95.0wt%；Melamine cyanurate is
4.0wt%；N tert octyl 2 benzothiazole sulfenamide is 1.0wt%.
The performance parameter of obtained flame resistant polyamide resin composition is：Flame retardant rating reaches UL94V-0, LOI after tested
It is 34.2% to be worth, and is 850 DEG C according to the GWIT of GB/T5169.13-2006 standard testings.
Embodiment 3
A kind of preparation method of flame resistant polyamide resin composition, by PA12, melamine N, N- diethyl -2- benzo thiophenes
Azoles sulfenamide and calcium stearate melting mixing are stirred, and flame resistant polyamide resin composition is obtained after cooling；Wherein melt
The temperature of mixing is 200 DEG C；The mode of cooling is cooled down for High Purity Nitrogen atmosphere, and the purity of nitrogen is 99.99% in High Purity Nitrogen atmosphere；
Each component percentage is as follows in flame resistant polyamide resin composition：Polyamide is 80.0wt%；Melamine is
15.0wt%；N, N- diethyl-2-benzothiazole sulfenamide are 4.5wt%；Calcium stearate is 0.5wt%.
The performance parameter of obtained flame resistant polyamide resin composition is：Flame retardant rating reaches UL94V-0, LOI after tested
It is 34.5% to be worth, and is 860 DEG C according to the GWIT of GB/T5169.13-2006 standard testings.
Embodiment 4
A kind of preparation method of flame resistant polyamide resin composition, by PA46, melamine phosphate, N- oxygen diethylene-
2-[4-morpholinodithio sulfenamide and zinc stearate melting mixing are stirred, and flame resistant polyamide resin composition is obtained after cooling；
Wherein the temperature of melting mixing is 180 DEG C；The mode of cooling is pure water cooling；Each component in flame resistant polyamide resin composition
Percentage is as follows：Polyamide is 85.0wt%；Melamine phosphate is 10wt%；N- oxygen diethylene -2-[4-morpholinodithio
Sulfenamide is 4.8wt%；Zinc stearate is 0.2wt%.
The performance parameter of obtained flame resistant polyamide resin composition is：Flame retardant rating reaches UL94V-0, LOI after tested
It is 34.5% to be worth, and is 855 DEG C according to the GWIT of GB/T5169.13-2006 standard testings.
Embodiment 5
A kind of preparation method of flame resistant polyamide resin composition, by PA6, melamine hypophosphite, N, the hexamethylenes of N- bis-
Mixture and the tristerin melting of base -2-[4-morpholinodithio sulfenamide and N tert butyl benzothiazole 2 sulfenamide
Mixing and stirring, obtains flame resistant polyamide resin composition after cooling.Wherein the temperature of melting mixing is 190 DEG C；Cooling
Mode is pure water cooling.Each component percentage is as follows in flame resistant polyamide resin composition：Polyamide is 75.0wt%；
Melamine hypophosphite is 18.0wt%；N, N- dicyclohexyl -2-[4-morpholinodithio sulfenamide and the N- tert-butyl group -2- benzo thiophenes
The mixture of azoles sulfenamide is 6.4wt%, wherein N in mixture, N- dicyclohexyls -2-[4-morpholinodithio sulfenamide and uncle N-
The mass ratio of butyl -2-[4-morpholinodithio sulfenamide is 2:1；Tristerin is 0.6wt%.
The performance parameter of obtained flame resistant polyamide resin composition is：Flame retardant rating reaches UL94V-0, LOI after tested
It is 34.8% to be worth, and is 865 DEG C according to the GWIT of GB/T5169.13-2006 standard testings.
Embodiment 6
A kind of preparation method of flame resistant polyamide resin composition, by PA66, melamine polyphosphate, N- cyclohexyl-
2-[4-morpholinodithio sulfenamide and ethylene stearic amide melting mixing are stirred, and flame resistant polyamide resin group is obtained after cooling
Compound.Wherein the temperature of melting mixing is 200 DEG C；The mode of cooling is cooled down for High Purity Nitrogen atmosphere.Flame resistant polyamide resin is combined
Each component percentage is as follows in thing：Polyamide is 90.0wt%；Melamine polyphosphate is 8.0wt%；N- cyclohexyl-
2-[4-morpholinodithio sulfenamide is 1.3wt%；Ethylene stearic amide is 0.7wt%.
The performance parameter of obtained flame resistant polyamide resin composition is：Flame retardant rating reaches UL94V-0, LOI after tested
It is 34.8% to be worth, and is 854 DEG C according to the GWIT of GB/T5169.13-2006 standard testings.
Embodiment 7
A kind of preparation method of flame resistant polyamide resin composition, by PA610, melamine borate salt, N- t-octyls -2-
Benzothiazole sulfenamide and erucyl amide melting mixing are stirred, and flame resistant polyamide resin composition is obtained after cooling.Its
The temperature of middle melting mixing is 190 DEG C；The mode of cooling is cooled down for High Purity Nitrogen atmosphere, and the purity of nitrogen is in High Purity Nitrogen atmosphere
99.99%.Each component percentage is as follows in flame resistant polyamide resin composition：Polyamide is 88wt%；Melamine boron
Hydrochlorate is 8wt%；N tert octyl 2 benzothiazole sulfenamide is 3.0wt%；Erucyl amide is 1.0wt%.
The performance parameter of obtained flame resistant polyamide resin composition is：Flame retardant rating reaches UL94V-0, LOI after tested
It is 34.4% to be worth, and is 853 DEG C according to the GWIT of GB/T5169.13-2006 standard testings.
Embodiment 8
A kind of preparation method of flame resistant polyamide resin composition, by PA612, melamine, N, N- diethyl -2- benzos
Thiazolesulfenamide and montanic acid sodium fusion melt mixing and stirring, and flame resistant polyamide resin composition is obtained after cooling.Wherein melt
The temperature for melting mixing is 260 DEG C；The mode of cooling is pure water cooling.Each component percentage in flame resistant polyamide resin composition
It is as follows：Polyamide is 83.0wt%；Melamine is 10.0wt%；N, N- diethyl-2-benzothiazole sulfenamide is
6.1wt%；Montanic acid sodium is 0.9wt%.
The performance parameter of obtained flame resistant polyamide resin composition is：Flame retardant rating reaches UL94V-0, LOI after tested
It is 34.6% to be worth, and is 850 DEG C according to the GWIT of GB/T5169.13-2006 standard testings.
Embodiment 9
A kind of preparation method of flame resistant polyamide resin composition, by PA1010, melamine, N, N- diisopropyls -2-
Benzothiazole sulfenamide and montanic acid sodium fusion melt mixing and stirring, and flame resistant polyamide resin composition is obtained after cooling.Its
The temperature of middle melting mixing is 200 DEG C；The mode of cooling is cooled down for High Purity Nitrogen atmosphere, and the purity of nitrogen is in High Purity Nitrogen atmosphere
99.99%.Each component percentage is as follows in flame resistant polyamide resin composition：Polyamide is 90wt%；Melamine is
7.0wt%；N, N- diisopropyl -2-[4-morpholinodithio sulfenamide are 2.7wt%；Montanic acid sodium is 0.3wt%.
The performance parameter of obtained flame resistant polyamide resin composition is：Flame retardant rating reaches UL94V-0, LOI after tested
It is 34.0% to be worth, and is 856 DEG C according to the GWIT of GB/T5169.13-2006 standard testings.
Comparative example 1
A kind of preparation method of flame resistant polyamide resin composition, it is identical with the preparation condition of embodiment 5, difference
It is that the fire retarding synergist that this comparative example is used is trithiocyanuric acid.
Obtained flame-proof PA 6 material as stated above, after tested flame retardant rating reach UL94V-0, LOI values are 32.0%,
According to GB/T5169.13-2006 standard testings, it is impossible to be 850 DEG C by GWIT and test.
Claims (7)
1. a kind of flame resistant polyamide resin composition, it is characterized in that：The component and content of the flame resistant polyamide resin composition
It is as follows：
The fire retarding synergist is one or more of sulfenamide compound；
Flame retardant rating reaches UL94V-0 to the flame resistant polyamide resin composition after tested；LOI value >=34.0%；According to GB/
Nonflammable temperature >=850 DEG C of T5169.13-2006 standard testings.
2. flame resistant polyamide resin composition according to claim 1, it is characterised in that the polyamide is nylon
6th, nylon 11, nylon 12, nylon 46, nylon66 fiber, NYLON610, nylon 612 or nylon 1010.
3. flame resistant polyamide resin composition according to claim 1, it is characterised in that the sulfenamide compound is
N, N- diethyl-2-benzothiazole sulfenamide, N- oxygen diethylene -2-[4-morpholinodithio sulfenamide, N, N- dicyclohexyl -2- benzene
And thiazolesulfenamide, N tert butyl benzothiazole 2 sulfenamide, N cyclohexyl 2 benzothiazole sulfenamide, N- are tertiary pungent
Base -2-[4-morpholinodithio sulfenamide or N, N- diisopropyl -2-[4-morpholinodithio sulfenamide.
4. flame resistant polyamide resin composition according to claim 1, it is characterised in that the melamine derivative is
Melamine cyanurate, melamine phosphate, melamine hypophosphite, melamine polyphosphate or melamine boron
Hydrochlorate.
5. flame resistant polyamide resin composition according to claim 1, it is characterised in that the processing aid is tristearin
Acid, calcium stearate, zinc stearate, tristerin, ethylene stearic amide, erucyl amide or montanic acid sodium.
6. the preparation method of the flame resistant polyamide resin composition as described in claim 1-5 is any, it is characterized in that：By polyamide
Resin, melamine or melamine derivative, the four kinds of material melts mixing of fire retarding synergist and processing aid, obtain after cooling
Flame resistant polyamide resin composition.
7. the preparation method of flame resistant polyamide resin composition according to claim 6, it is characterised in that the melting is mixed
The temperature of conjunction is 150-290 DEG C；The mode of the cooling is that pure water or High Purity Nitrogen atmosphere are cooled down；Nitrogen in the High Purity Nitrogen atmosphere
Purity >=99.9% of gas.
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| CN107418201A (en) * | 2017-08-30 | 2017-12-01 | 惠州市华聚塑化科技有限公司 | A kind of efficient halogen-free anti-inflaming enhancing nylon composite materials and preparation method thereof |
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Application publication date: 20170524 |