CN103351618A - Antistatic, halogen-free, and fire-retardant enhanced master batch dedicated for polyamide and preparation method thereof - Google Patents
Antistatic, halogen-free, and fire-retardant enhanced master batch dedicated for polyamide and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an antistatic, halogen-free, and fire-retardant enhanced master batch dedicated for polyamide and a preparation method thereof. The fire-retardant master batch is composed of following components in parts by weight: 25 to 50 parts of PA, 15 to 30 parts of alkyl phosphinate fire-retardant, 15 to 30 parts of melamine polyphosphate fire retardant, 8 to 15 parts of zinc borate fire retardant, 4 to 6 parts of CTI improver, 1 to 1.5 parts of antistatic agent, 3 to 8 parts of flexibilizer, 0.5 to 1 part of coupling agent, 0.7 to 1.5 parts of lubricant, and 0.3 to 1 part of anti-oxidant. The sum of the weight ratio of components mentioned above is 100 wt%. The fire-retardant master batch is used to produce fire-retardant enhanced and modified nylon, meets standards of the United States underwriters laboratories (UL)-941.6mm and a higher V-0 grade, simultaneously achieves that glowing wire temperature (GWIT) is equal to or larger than 750 DEG C and the CTI value is equal to or larger than 600 V, also has a antistatic performance, meets European Union RoHS, International Electrotechnical Commission (IEC) halogen-free and Reach rule requirements, is easy to use and excellent in comprehensive performance, and does not affect color matching.
Description
Technical field
The present invention relates to the flame-retardant modified field of macromolecular material, especially relate to the special-purpose anti-static halogen-free flame-retardant of a kind of novel polyamide and strengthen master batch and preparation method thereof.
Background technology
Nylon is a kind of excellent property, of many uses, large usage quantity cross engineering plastics, it is widely used in the fields such as electric, transportation building, vehicle manufacturing, office appliance, sports equipment, have excellent over-all properties: intensity is high, toughness is better (hygrometric state); Oil resistant, organic solvent-resistant, chemical resistance are good; Frictional coefficient is little, and self-lubricating property is good; Good processability.Along with electric and signal equipment develop towards miniaturization, lightweight, high performance, the consumption of modified nylon material is increasing.But nylon also exists weak point, and pure nylon intensity is relatively poor, and heat-drawn wire is low, size is unstable, inflammableness, and easily suction waits the popularization that has limited again in every field, so generally nylon is carried out fire-retardant, enhancing modified, to adapt to its more high strength requirement and fire-retardant requirement.Glass fiber enhanced nylon has the advantages such as intensity is high, good stability of the dimension and is used widely.For glass fiber enhanced nylon, because " the candle wick effect " of glass fibre makes more easy firing of material.So be the direction that everybody studies to the flame-retardant modified of it always.
Fire retardant about the glass fiber enhanced nylon matrix material mostly is greatly halogen flame retardant at present, but the enforcement along with the RoHS of European Union and WEEE instruction, and the enhancing of people's environmental consciousness, material requirements to plastic prod is also more and more higher, when particularly fire retardant material uses, require material both to have superperformance, while environmental pollution and light to the mankind's harm, traditional like this halogen flame retardant can't reach this requirement, although halogen flame has improved the flame retardant resistance of material to a certain extent, but the mechanical property of material and electrical insulation capability all are greatly affected, (CTI) drops to 250V even lower from 600V such as phase ratio creepage tracking index, directly affected the application of material at electronic enterprises.Halogen-free flameproof becomes the inexorable trend of flame-retardant modified development, so the glass fiber enhanced nylon matrix material uses the exploitation of Halogen precipitate-free flame retardant agent to become the focus of current research.
The fire retardant of halogen-free flame-retardant reinforced nylon commonly used is OP1312 and the OP1311 of German Ke Laien in the market, complete dependence on import, price Ao Gui, the supply of material is unstable, and the fire retardant addition is large, and is powder, the price difficulty has higher requirement to board and technique.Again because flame-retardant reinforced nylon has high-ohmic, so that nylon product contacts with other materials or when rubbing, be easy to produce static and constantly accumulation, after strengthening simultaneously since surfaceness increase, can strengthen accumulation of static electricity, thereby can produce a series of potential safety hazard because of static.
Summary of the invention
The object of the present invention is to provide a kind ofly to have that processing is stable, mechanical property is high, flame retardant properties is stable, and the special-purpose anti-static halogen-free flame-retardant of the polymeric amide of permanent antistatic strengthens master batch and preparation method thereof.
Another object of the present invention is to provide the special-purpose anti-static halogen-free flame-retardant of a kind of polymeric amide to strengthen the preparation method of master batch.
For reaching above-mentioned purpose, the present invention is achieved by the following technical solutions: the special-purpose anti-static halogen-free flame-retardant of a kind of polymeric amide strengthens master batch, comprises that following component and each weight percentages of components (wt%) are: PA:25-50; Alkyl phosphinate fire retardant: 15-30; Melamine polyphosphate fire retardant: 15-30; Zinc borate flame retardant: 8-15; CTI improving agent: 4-6; Static inhibitor: 1-1.5; Toughner: 3-8; Lubricant: 0.7-1.5; Oxidation inhibitor: 0.3-1.It is 100% that above-mentioned each component satisfies the weight proportion sum.
Described nylon be for low sticking or in sticking PA6 or PA66, be respectively the PA6-TP4208 that the Taiwan collection is contained, the PA66-50BWFS of the first promise of the U.S. can guarantee that like this processing fluidity is better.
Described alkyl phosphinate fire retardant is that diethyl phospho acid aluminium, methylethyl phospho acid aluminium are composite according to the quality proportioning of 2:1.
Described melamine polyphosphate is the MPP through special modification, with the consistency of increase with PA.
Described zinc borate flame retardant is the commercially available general zinc borate that contains 3.5 crystal water.
Described CTI improving agent is that calcium oxide, Magnesium Stearate, talcum powder are composited according to the quality proportioning of 3:1:1.
Described static inhibitor is that anionic, non-ionic type are composite according to massfraction 2:1.
Described silane coupling agent is the silane coupling agent of epoxy group(ing).
Described toughner is that EPDM-g-MAH and Acrylate-g-POE-g-MAH are composite according to massfraction 2:1.
Described lubricant is the silicone powder; Described oxidation inhibitor is that to be that 1:2 is composite according to weight ratio form for phenolic antioxidant 1010 and phosphoric acid ester irgasfos 168.
The special-purpose anti-static halogen-free flame-retardant of polymeric amide strengthens the preparation method of master batch, and it is characterized in that: its preparation method may further comprise the steps:
(1) takes by weighing each component by weight percent claimed in claim 1;
(2) take by weighing first the PA resin, silane coupling agent is put into homogenizer stirring at low speed 2min, then above-mentioned fire retardant and other auxiliary agents being taken by weighing according to proportion places the homogenizer high speed to stir 5min, the raw material that stirs is changed in the twin screw extruder, through frit reaction, extruding pelletization;
(3) twin screw extruder is respectively distinguished temperature and is controlled at respectively 210-270 degree centigrade, and seven districts vacuumize, and screw speed is 350-450r/min, and employed screw combinations is optimized screw combinations.
The present invention provides the special-purpose anti-static halogen-free flame-retardant of a kind of polymeric amide to strengthen master batch and preparation method thereof, and modified effect is good, uses simply, can join shades of colour, and antistatic effect is good, meets simultaneously ROHS, IEC and the Reach laws and regulations requirement of European Union.Further promote halogen-free flame-retardant reinforced nylon in the application in the fields such as electric, transportation building, vehicle manufacturing, office appliance, sports equipment for promoting.
Embodiment
Embodiment one
The special-purpose anti-static halogen-free flame-retardant of a kind of novel polyamide strengthens the preparation of master batch, and this halogen-free flame-retardant master batch forms (wt%) by following raw materials according according to mass parts:
PA 28%, alkyl hypophosphite 25%, melamine polyphosphate 25%, zinc borate 25%, CTI promotor 5%, toughner 4%, lubricant 0.7%, oxidation inhibitor 0.3%, static inhibitor 1.2%, silane coupling agent 0.8%; Said mixture is added to twin screw extruder, frit reaction, extruding pelletization strengthens master batch thereby make the special-purpose anti-static halogen-free flame-retardant of novel polymeric amide.
Embodiment two
The special-purpose anti-static halogen-free flame-retardant of the polymeric amide of above-mentioned preparation is strengthened master batch, add among the PA6, carry out the fiberglass reinforced fire retardant modification, this anti-static halogen-free flame-retardant strengthens PA6 and is comprised of following starting material, and its mass parts (wt%) proportioning is respectively:
PA6 43.5%, silane coupling agent 0.5%, alkali-free glass fiber yarn 30%, the special-purpose anti-electrostatic fire retardant of polymeric amide strengthen master batch 25%, oxidation inhibitor 0.3%, lubricant 0.7%; Said mixture is added to twin screw extruder, frit reaction, extruding pelletization descended dry 4-6 hour at 110 ℃-120 ℃, required to be injection molded into the standard batten according to GB, carried out performance test.
Embodiment three
The special-purpose anti-static halogen-free flame-retardant of the polymeric amide of above-mentioned preparation is strengthened master batch, add among the PA66, carry out the fiberglass reinforced fire retardant modification, this anti-static halogen-free flame-retardant reinforced plastic PA66 is comprised of following starting material, and its mass parts (wt%) proportioning is respectively:
PA66 43.5%, silane coupling agent 0.5%, alkali-free glass fiber yarn 30%, the special-purpose anti-electrostatic fire retardant of polymeric amide strengthen master batch 25%, oxidation inhibitor 0.3%, lubricant 0.7%; Said mixture is added to twin screw extruder, frit reaction, extruding pelletization descended dry 4-6 hour at 110 ℃-120 ℃, required to be injection molded into the standard batten according to GB, carried out performance test.
The performance test results of embodiment 2 and embodiment 3 is as shown in the table:
| Test event | Testing standard | Test condition | Anti-static halogen-free flame-retardant strengthens PA6 | The anti-static halogen-free flame-retardant reinforced plastic PA66 |
| Tensile strength MPa | GB 1040 | 10mm/min | 140 | 155 |
| Elongation % | GB 1040 | 10mm/min | 3 | 3 |
| Modulus in flexure MPa | GB 9341 | 2mm/min | 180 | 190 |
| Flame retardant test | UL94 | 1.6mm | V0 | V0 |
| Surface resistivity Ω | GB1410 | / | 5.8*10 8 | 6.7*10 8 |
| Socle girder notched Izod impact strength kj/cm 2 | GB 1843 | 4J | 16 | 14 |
| Heat-drawn wire ℃ | GB 1634 | 1.82Mpa | 220 | 245 |
| Glowing filament ℃ | GB 5169 | 750 | OK | OK |
| CTI tests V | GB 4702 | 600 | OK | OK |
Comprehensive upper table can be found out, the preparation alloy that the special-purpose anti-static halogen-free flame-retardant of a kind of polymeric amide of the present invention strengthens master batch have process, flame retardant effect obviously, permanent antistatic, characteristics that mechanical property is higher, and cost is moderate, is a kind of high comprehensive performance, the master batch that cost performance is high.The embodiment that the present invention is better, all changes of having done according to technical solution of the present invention when the function that produces fails to exceed the scope of technical solution of the present invention, all belong to protection scope of the present invention.
Claims (9)
1. the special-purpose anti-static halogen-free flame-retardant of polymeric amide strengthens master batch, and it is characterized in that: this master batch comprises following component and weight part content (wt%):
PA：25-50；
Alkyl phosphinate fire retardant: 15-30;
Melamine polyphosphate fire retardant: 15-30;
Zinc borate flame retardant: 8-15;
CTI improving agent: 4-6;
Static inhibitor: 1-1.5;
Coupling agent: 0.5-1;
Toughner: 3-8;
Lubricant: 0.7-1.5;
Oxidation inhibitor: 0.3-1.
2. the special-purpose anti-static halogen-free flame-retardant of a kind of polymeric amide according to claim 1 strengthens master batch, it is characterized in that: described PA for low sticking or in sticking PA6 or PA66.
3. the special-purpose anti-static halogen-free flame-retardant of a kind of polymeric amide according to claim 1 strengthens master batch, it is characterized in that: described alkyl phosphinate fire retardant is that in hydroxymethyl phenyl phospho acid aluminium, diethyl phospho acid aluminium, the methylethyl phospho acid aluminium one or more are composite.
4. the special-purpose anti-static halogen-free flame-retardant of a kind of polymeric amide according to claim 1 strengthens master batch, it is characterized in that: described melamine polyphosphate fire retardant is the MPP through special modification.
5. the special-purpose anti-static halogen-free flame-retardant of a kind of polymeric amide according to claim 1 strengthens master batch, and it is characterized in that: described zinc borate flame retardant is the zinc borate that contains 3.5 crystal water.
6. the special-purpose anti-static halogen-free flame-retardant of a kind of polymeric amide according to claim 1 strengthens master batch, it is characterized in that: described CTI improving agent is that calcium oxide, Magnesium Stearate, talcum powder are composited according to the quality proportioning of 3:1:1.
7. the special-purpose anti-static halogen-free flame-retardant of a kind of polymeric amide according to claim 1 strengthens master batch, it is characterized in that: described static inhibitor is that in cationic, anionic or the non-ionic antistatic agent one or more are composite.
8. the special-purpose anti-static halogen-free flame-retardant of a kind of polymeric amide according to claim 1 strengthens master batch, and it is characterized in that: described coupling agent is silane coupling agent, a kind of in amino silicane coupling agent or the epoxy silane coupling; Described toughner is POE-g-MAH, EPDM-g-MAH or Acrylate-g-POE-g-MAH; : described lubricant is one or more in EBS, PETS or the silicone powder; Described oxidation inhibitor is that to be that 1:2 is composite according to weight ratio form for phenolic antioxidant 1010 and phosphoric acid ester irgasfos 168.
9. the special-purpose anti-static halogen-free flame-retardant of a kind of polymeric amide according to claim 1 strengthens the preparation method of master batch, and it is characterized in that: its preparation method may further comprise the steps:
(1) takes by weighing each component by weight percent claimed in claim 1;
(2) take by weighing first the PA resin, silane coupling agent is put into homogenizer stirring at low speed 2min, then above-mentioned fire retardant and other auxiliary agents being taken by weighing according to proportion places the homogenizer high speed to stir 5min, the raw material that stirs is changed in the twin screw extruder, through frit reaction, extruding pelletization;
(3) twin screw extruder is respectively distinguished temperature and is controlled at respectively 210-270 degree centigrade, and seven districts vacuumize, and screw speed is 350-450r/min, and employed screw combinations is optimized screw combinations.
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| CN103627168A (en) * | 2013-11-13 | 2014-03-12 | 广东聚石化学股份有限公司 | Special halogen-free flame-retardant master batch for nylon and preparation method thereof |
| CN105504657A (en) * | 2016-01-07 | 2016-04-20 | 苏州法斯特信息科技有限公司 | Flame-retardant antistatic ABS composite material and preparation method thereof |
| CN107629450A (en) * | 2017-10-16 | 2018-01-26 | 中山康诺德新材料有限公司 | A kind of environment friendly non-halogen type fiber glass reinforced polyamide fire retardant |
| CN108291050A (en) * | 2015-11-26 | 2018-07-17 | 科莱恩塑料和涂料有限公司 | Polymer-type flame-retardant mixture |
| CN109694568A (en) * | 2017-10-24 | 2019-04-30 | 广州市寅源新材料科技有限公司 | A kind of High glow wire halogen-free flame retardant polyamide compound and the preparation method and application thereof |
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Application publication date: 20131016 |