CN106700525A - High-impact halogen-free flame-retardant POK/PA (polyketone/polyamide) alloy material - Google Patents
High-impact halogen-free flame-retardant POK/PA (polyketone/polyamide) alloy material Download PDFInfo
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/17—Component parts, details or accessories; Auxiliary operations
- B29C45/76—Measuring, controlling or regulating
- B29C45/78—Measuring, controlling or regulating of temperature
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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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
- C08L73/00—Compositions of macromolecular compounds obtained by reactions forming a linkage containing oxygen or oxygen and carbon in the main chain, not provided for in groups C08L59/00 - C08L71/00; Compositions of derivatives of such polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
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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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention relates to the field of high-polymer materials, and particularly relates to a high-impact halogen-free flame-retardant POK/PA (polyketone/polyamide) alloy material. The alloy material is composed of the following components in parts by weight: 200-400 parts of POK, 400-700 parts of PA6, 10-100 parts of compatibility and impact modifier, 50-150 parts of halogen-free flame retardant and 5-15 parts of aid. The high-impact halogen-free flame-retardant POK/PA alloy material has favorable high-impact properties (up to 250 J/M at 23 DEG C and up to 150 J/M at -30 DEG C); the halogen-free flame retardancy can reach V-0; the abrasion coefficient of the material is better than that of the simple flame-retardant PA6, and is up to 6.9 mm<3>/kg/km; and the heat-deformation temperature of the material is higher than that of the simple flame-retardant PA6, and is up to 190 DEG C.
Description
Technical field
It is a kind of HI high impact halogen-free flameproof POK/PA alloy materials specifically the present invention relates to polymeric material field.
Background technology
Polyamide (PA6) has the characteristics, one such as thermoplasticity, lightweight, excellent mechanical performance, chemicals-resistant and good endurance
As for the product such as auto parts and components, mechanical part, electric equipment products, engineering accessory.Have the disadvantage that water absorption rate is high, dry and tide
Strength difference is larger under wet environment, and notch shock is not high, and wearability is general, and shrinkage factor is larger etc..
Polyketone (POK) is the novel green polymeric material synthesized by carbon monoxide, alkene (ethene, propylene), molecule master
Chain is by hydrocarbon by the highly crystalline engineering plastics for forming close crystalline structure, excellent chemical resistance, shock resistance, frictional property
Energy and high barrier, compared with nylon, its shock resistance is eager to excel 3 times, and the stability to chemical substance is also significantly improved, surface
Hardness is also better than POM, can be used for automobile, electronics, the parts of industry material.But the simple POK ranges of work are narrow, to shaping
Frock and technological requirement are higher so that application is greatly limited, and experiment finds, the alloy surface wearability of POK and PA6
Significantly improved than PA6, the strength ratio PA6 of wet environment is substantially high, the more simple POK of processing temperature has and substantially widens.Consideration is got home
Electricity and electronic apparatus have flame-retardancy requirements, but POK/PA alloys improvement anti-flammability is rarely reported at present, and halogen-free flameproof is even more not to be had.
Nitrogenated flame retardant has Halogen, low toxicity, good stability, flame retarding efficiency high, the advantage such as environmentally friendly, 20th century 90
It has been developed rapidly since age.At present, it is mainly melamine and its derivative using more nitrogenated flame retardant
(MCA).The product of the fire-retardant burnings of MCA will not carry controversial halide and phosphorus system product, and its main component is CO, NH3
Deng material.MCA has an excellent high temperature resistant processing characteristics, and less than 300 DEG C are heated highly stable, and 350 DEG C start distillation, but regardless of
Solution.Generation melamine and cyanuric acid can be just decomposed in 440-450 DEG C of temperature, the work for absorbing heat and cooling thermal source is played
With.And the melamine that has gasified provides inertia source of the gas, can dilution oxygen and the fuel gas that is produced because high polymer is decomposed it is dense
Degree, so as to reach fire-retardant purpose.MCA non-volatile components at 300 DEG C, and solubility is low in water.When this fire retardant burns
Release nitrogen oxides, in the absence of the phenomenon that highly acid material is produced after hydrogen halides and phosphorus flame retardant burning, so because of its environmental protection
Characteristic and widely used in PA6.
Number of patent application 98121442.8《Polyketone flame retardant composition》Use trimeric-cyanamide cyanurate fire-retardant merely
POK, anti-flammability can only achieve V-2, and be not directed to the assessment of fire proofing mechanical performance.
A kind of HI high impact halogen-free flameproof POK/PA alloy materials how are developed, is worth constantly inquiring into and studying.At present, not yet
See the relevant report of PA/POK alloy fire proofings, halogen-free flameproof is even more not to be had.
The content of the invention
It is an object of the invention to provide a kind of HI high impact halogen-free flameproof POK/PA alloy materials, can be applicable to it is fire-retardant and
The plug for industrial use of wear-resisting requirement, geared parts, and cold district low temperature requirements outdoor industry accessories.
The first aspect of the present invention, there is provided a kind of HI high impact halogen-free flameproof POK/PA alloy materials, by following component by such as
Lower weight portion composition：
Wherein, the polyketone POK is the copolymer of carbon monoxide and alkene, and number-average molecular weight is 10000-100000；Institute
It is that, by the nylon 6 of caprolactam open loop polycondensation, number-average molecular weight is 16000-33000 to state nylon PA 6；The compatible impact changes
Property agent for core shell structure silicon-acrylate-epoxide modified polymer, with silicon rubber-acrylate composite rubber as core, poly- first
Base glycidyl acrylate (GMA) is the graft copolymer of the core shell structure of shell.
Further, the alkene is the mixture of ethene, propylene or both.
Further, the polyketone POK is carbon monoxide, ethene, the copolymer of propylene, and number-average molecular weight is 60000-
90000。
Further, the number-average molecular weight of the nylon PA6 is 20000-30000.Further, the halogen-free flame retardants
It is melamine cyanurate.
Further, the auxiliary agent includes the following components of percentage meter by weight：Antioxidant 20-30%, ultraviolet addition
Agent 30-35%, processing aid 30-35% and toner 8-10%.
Further, the antioxidant is selected from phosphite antioxidant 168, hindered phenol antioxygen 1010, hindered phenol antioxygen
One or two mixing in agent 1098, hindered phenol antioxygen 1076；Preferably, the antioxidant is irgasfos 168 and resists
The mixing of oxygen agent 1098.
Further, the antiultraviolet additive compares 1 for weight:1 light stabilizer and the compounding of ultra-violet absorber
Thing；Preferably, the light stabilizer is that light stablizes 770 or one kind for stablizing in 622 of light；The ultra-violet absorber be UV234,
In UV-328 or UV-320；It is furthermore preferred that the antiultraviolet additive is the compound that light stablizes 770 and UV-234.
Further, the processing aid is selected from Tissuemat E, OPE, pentaerythritol stearate, long-chain
One or more mixing in aliphatic acid polyfunctional group ester.Preferably, the processing aid is Tissuemat E.
Further, the toner is mainly made up of pigment and spread powder.
The second aspect of the present invention, there is provided the preparation method of above-mentioned HI high impact halogen-free flameproof POK/PA alloy materials, including
Following steps：
Raw material is weighed by described component ratio, all raw materials are dry-mixed 3-5 minutes at room temperature in super mixer,
Then at 220~240 DEG C through double screw extruder extrusion, cooling, granulation, gained pellet through after 100 DEG C of dryings 4 hours
Standard sample bar is molded at 240~260 DEG C, is obtained final product.
The compatible impact modifying agent that the present invention is used, the GMA epoxy polymers in structure improve the compatible of PA6 and POK
Property, while silicon rubber-acrylate composite rubber improves the normal temperature and low-temperature flexibility of material, silicon rubber therein grinds to reducing
Consumption coefficient also has certain synergy.
The invention has the advantages that：
1st, material has good high impact property (23 DEG C can reach 250J/M；- 30 DEG C can reach 150J/M), and
Halogen-free flameproof can reach V-0.
2nd, the barasion coefficient of material is better than simple flame-proof PA 6, reaches 6.9mm3/kg/km。
3rd, the heat distortion temperature of material is higher than simple flame-proof PA 6, reaches 190 DEG C.
Specific embodiment
The specific embodiment that the present invention is provided is elaborated with reference to embodiment.
In following each embodiment, each raw material uses following compositions：
1st, polyketone POK：There is provided by Hyosung group of South Korea, model M630A；
2nd, nylon PA 6：Using the PA6 by caprolactam open loop polycondensation, provided by Honeywell Inc., model
H8202NLB；
3rd, compatible impact modifying agent：There is provided by Mitsubishi Li Yang companies, model S2200 is (with silicon rubber-acrylate
Compounded rubber is core, and poly (glycidyl methacrylate) is the graft copolymer of the core shell structure of shell)；
4th, melamine cyanurate based flame retardant：There is provided by Hangzhou JLS Flame Retardants Chemical Co., Ltd., model
JLS-MC810；
5th, irgasfos 168, antioxidant 1098：Manufactured by BASF AG；
6th, light stablizes 770, ultra-violet absorber UV234：Manufactured by BASF AG；
7th, flow promortor is processed：Tissuemat E, OPE by BASF AG manufacture, pentaerythritol stearate by
Long Sha companies of the U.S. are manufactured, and LCFA polyfunctional group ester is manufactured by German Kening Co., Ltd.
Embodiment 1
By following component in parts by weight：
Above-mentioned raw materials component is mixed 3-5 minutes in high-speed mixer, is then squeezed through twin-screw at 220~240 DEG C
Go out machine extrusion, cooling, granulation, gained pellet is molded into standard sample bar after 4 hours through 100 DEG C of dryings at 240~260 DEG C, i.e.,
.
Embodiment 2-6
Raw material is weighed by the parts by weight in table 1, preparation method is with embodiment 1.
The component and proportioning of the embodiment 1-6 of table 1
The evaluation of implementation result
The sample that above-described embodiment 1 is obtained to embodiment 6, according to American Society Testing and Materials (ASTM) standard testing
Mechanical property, optical property, according to UL94 standard testing fire resistances, according to the abrasion system of GB 3960-83 Standards for Testing Materials
Number, test result is as shown in table 2 below：
The test result of the embodiment 1-6 of table 2
| Performance parameter | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Density (g/cm3) | 1.18 | 1.27 | 1.22 | 1.20 | 1.18 | 1.17 |
| Melt flow rate (MFR) (g/10min) | 20 | 9 | 18 | 15 | 13 | 13 |
| Elongation at break (%) | 17% | 220% | 65% | 79% | 102% | 125% |
| Tensile strength (MPa) is dried | 75 | 70 | 72 | 68 | 65 | 62 |
| Tensile strength (MPa) is moistened | 50 | 62 | 58 | 61 | 59 | 56 |
| Bending modulus (MPa) is dried | 3000 | 2200 | 2850 | 2700 | 2550 | 2400 |
| Bending modulus (MPa) is moistened | 1700 | 2050 | 1950 | 2200 | 2250 | 2200 |
| 23 DEG C of lzod notch impact strengths (J/m) | 52 | 145 | 73 | 150 | 250 | 300 |
| - 30 DEG C of lzod notch impact strengths (J/m) | 35 | 89 | 38 | 96 | 150 | 180 |
| Heat distortion temperature (DEG C) 0.45MPa | 180 | 210 | 196 | 193 | 190 | 188 |
| Anti-flammability | V-0 | V-2 | V-0 | V-0 | V-0 | V-2 |
| Barasion coefficient (mm3/kg/km) | 12 | 0.6 | 7.8 | 7.3 | 6.9 | 6.8 |
The test performance result of table 2 shows：
(1) obtained from the analysis of embodiment 1~3, MCA is used in pure polyketone material, and flame retardant effect is poor, but in PA/POK
Flame retardant rating can be made V-0 grades is reached in alloy.Also, the addition of POK, reduces sensitiveness of the PA6 to moisture, reduces PA6
Barasion coefficient, improve the heat distortion temperature of PA6.
(2) obtained from the analysis of embodiment 4~6, the addition of compatible impact modifying agent S2200, the GMA epoxide polymerizations in structure
Thing improves the compatibility of PA6 and POK, while normal temperature and low temperature that silicon rubber-acrylate composite rubber improves material are tough
Property, and as addition increases, toughness substantially increases, barasion coefficient reduction.But more than 10% is reached in addition, anti-flammability is bright
It is aobvious to decline, V-0 requirements cannot have been met.Therefore the optimum addition of compatible impact modifying agent S2200 is in the 8% (conjunction of embodiment 5
Golden material combination property is optimal).
Below the preferred embodiment to the invention is illustrated, but the invention be not limited to it is described
Embodiment, those of ordinary skill in the art can also make a variety of equivalent on the premise of without prejudice to the invention spirit
Modification or replacement, these equivalent modifications or replacement are all contained in the application claim limited range.
Claims (7)
1. a kind of HI high impact halogen-free flameproof POK/PA alloy materials, are made up of following component by following weight portion：
Wherein, the polyketone POK is the copolymer of carbon monoxide and alkene, and alkene is the mixture of ethene, propylene or both,
Ketone POK number-average molecular weights are 10000-100000；The nylon PA 6 is that, by the nylon 6 of caprolactam open loop polycondensation, number is divided equally
Son amount is 16000-33000；The compatible impact modifying agent is the silicon-acrylate-epoxide modified polymer of core shell structure, with
Silicon rubber-acrylate composite rubber is core, and poly (glycidyl methacrylate) is the graft copolymer of the core shell structure of shell.
2. a kind of HI high impact halogen-free flameproof POK/PA alloy materials according to claim 1, it is characterised in that：The polyketone
POK is carbon monoxide, ethene, the copolymer of propylene, and number-average molecular weight is 60000-90000.
3. a kind of HI high impact halogen-free flameproof POK/PA alloy materials according to claim 1, it is characterised in that：The nylon
The number-average molecular weight of PA 6 is 20000-30000.
4. a kind of HI high impact halogen-free flameproof POK/PA alloy materials according to claim 1, it is characterised in that：The Halogen
Fire retardant is melamine cyanurate.
5. a kind of HI high impact halogen-free flameproof POK/PA alloy materials according to claim 1, it is characterised in that：The auxiliary agent
Following components including percentage meter by weight：Antioxidant 20-30%, ultraviolet additive 30-35%, processing aid 30-35%
With toner 8-10%.
6. a kind of HI high impact halogen-free flameproof POK/PA alloy materials according to claim 5, it is characterised in that：The antioxygen
Agent is selected from phosphite antioxidant 168, hindered phenol antioxygen 1010, hindered phenol antioxygen 1098, hindered phenol antioxygen 1076
One or two mixing；The antiultraviolet additive compares 1 for weight:1 light stabilizer and ultra-violet absorber are answered
With thing；It is multifunctional that the processing aid is selected from Tissuemat E, OPE, pentaerythritol stearate, LCFA
The mixing of one or more in group's ester.
7. the preparation method of a kind of HI high impact halogen-free flameproof POK/PA alloy materials according to claim any one of 1-6,
Comprise the following steps：
Raw material is weighed by described component ratio, all raw materials are dry-mixed 3-5 minutes at room temperature in super mixer, then
Through double screw extruder extrusion, cooling, granulation at 220~240 DEG C, gained pellet through after 100 DEG C of dryings 4 hours 240~
Standard sample bar is molded at 260 DEG C, is obtained final product.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107189402A (en) * | 2017-07-07 | 2017-09-22 | 东莞市卡帝德塑化科技有限公司 | Modified engineered plastic material and preparation method for manufacturing lithium cell core shell |
| CN107189420A (en) * | 2017-06-14 | 2017-09-22 | 上海长伟锦磁工程塑料有限公司 | A kind of low warpage POK PA alloy materials of high wear-resistance anti-static |
| CN109608878A (en) * | 2018-12-13 | 2019-04-12 | 上海长伟锦磁工程塑料有限公司 | A kind of halogen-free flameproof enhancing PA/POK alloy material of wet and heat ageing resistant |
| CN113480807A (en) * | 2021-05-27 | 2021-10-08 | 广州辰东新材料有限公司 | Polyamide, polyketone and polyolefin alloy material and preparation method thereof |
| CN114656744A (en) * | 2022-05-20 | 2022-06-24 | 广东乔艺塑胶有限公司 | Low-odor PP/AS/POK ternary composite resin, cosmetic packaging material and preparation method thereof |
| WO2024041953A1 (en) | 2022-08-23 | 2024-02-29 | Basf Se | Flame retardant polyamide composition and article produced from the composition |
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| CN105885398A (en) * | 2016-01-25 | 2016-08-24 | 南京德尔隆工程塑料有限公司 | Hydrolysis-resistant polyamide composite and preparation method thereof |
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| WO1999055782A1 (en) * | 1998-04-29 | 1999-11-04 | Bp Chemicals Limited | Polymer blends from polyketone and polyamide |
| CN101023137A (en) * | 2004-09-21 | 2007-08-22 | Ems化学股份公司 | Use of stabilized thermoplastic polyamide molding compounds as a coating for optical waveguides |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107189420A (en) * | 2017-06-14 | 2017-09-22 | 上海长伟锦磁工程塑料有限公司 | A kind of low warpage POK PA alloy materials of high wear-resistance anti-static |
| CN107189420B (en) * | 2017-06-14 | 2019-09-27 | 上海长伟锦磁工程塑料有限公司 | A kind of low warpage POK-PA alloy material of high wear-resistance anti-static |
| CN107189402A (en) * | 2017-07-07 | 2017-09-22 | 东莞市卡帝德塑化科技有限公司 | Modified engineered plastic material and preparation method for manufacturing lithium cell core shell |
| CN109608878A (en) * | 2018-12-13 | 2019-04-12 | 上海长伟锦磁工程塑料有限公司 | A kind of halogen-free flameproof enhancing PA/POK alloy material of wet and heat ageing resistant |
| CN109608878B (en) * | 2018-12-13 | 2021-06-04 | 上海长伟锦磁工程塑料有限公司 | Damp-heat-aging-resistant halogen-free flame-retardant reinforced PA/POK alloy material |
| CN113480807A (en) * | 2021-05-27 | 2021-10-08 | 广州辰东新材料有限公司 | Polyamide, polyketone and polyolefin alloy material and preparation method thereof |
| CN114656744A (en) * | 2022-05-20 | 2022-06-24 | 广东乔艺塑胶有限公司 | Low-odor PP/AS/POK ternary composite resin, cosmetic packaging material and preparation method thereof |
| CN114656744B (en) * | 2022-05-20 | 2022-07-29 | 广东乔艺塑胶有限公司 | Low-odor PP/AS/POK ternary composite resin, cosmetic packaging material and preparation method thereof |
| WO2024041953A1 (en) | 2022-08-23 | 2024-02-29 | Basf Se | Flame retardant polyamide composition and article produced from the composition |
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