CN103160113A - Halogen-free flame-retardant antibacterial PET / PA6 alloy material and preparation method thereof - Google Patents
Halogen-free flame-retardant antibacterial PET / PA6 alloy material and preparation method thereof Download PDFInfo
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- CN103160113A CN103160113A CN2011104190961A CN201110419096A CN103160113A CN 103160113 A CN103160113 A CN 103160113A CN 2011104190961 A CN2011104190961 A CN 2011104190961A CN 201110419096 A CN201110419096 A CN 201110419096A CN 103160113 A CN103160113 A CN 103160113A
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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
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
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Abstract
The invention relates to a halogen-free flame-retardant antibacterial PET / PA6 alloy material and a preparation method thereof. The material comprises the following components by weight: 10-30 parts of PET, 640-70 parts of PA, 0.1-0.6 part of an antioxidant, 0.1-1 part of a lubricant, 0.01-0.1 part of a compatibilizer, 5-8 parts of a phosphorus system flame retardant, 1-8 parts of a nitrogen system flame retardant, 0.2-3 parts of an antibacterial agent, and 10-30 parts of a mineral powder. The product is prepared by drying polyethylene terephthalate PET and polytrimethylene terephthalate PA6, mixing with the prepared lubricant, antioxidant, compatibilizer and flame retardant, and conducting extrusion granulation, water cooling, sized dicing and drying. Compared with the prior art, the invention has the advantages of simple and reasonable process, safety and environment protection.
Description
Technical field
The present invention relates to a kind of polymer composite, especially relate to a kind of antimicrobial halogen-free flame PET/PA6 alloy material and preparation method thereof.
Background technology
Polycaprolactam (PA6) has that mechanical strength is high, softening temperature is high, impelling strength is good, heat-resisting, solvent-proof advantage, but price comparison is high.Polyethylene terephthalate (PET) is kind important in thermoplastic polyester, and anti-creep and fatigue property are good, and surface hardness is high, and price is low.PET and PA6 are made alloy material can make system possess good thermotolerance, solvent resistance and mechanical property, and can reduce costs.
At present, improving one of effective means of plastic material flame retardant properties is to add bromo-antimony compound system fire retardant.This system good flame retardation effect, addition are low, little to the Effect on Mechanical Properties of material, but discharge objectionable impuritiess such as producing hydrogen bromide when burning due to it, health and environment to people all can cause greatly harm, electrical property impact on material is very large, so its range of application more and more is restricted.Parliament of European Union and EU Council passed through No. 2002/95/EC " ROHS " on January 23rd, 2003, limit the application of some brominated flame-retardant in electronic and electrical equipment, thus the without halide fire retardant material of high flame retardant, high safety, low toxicity, low cigarette, non-corrosiveness γ-ray emission oneself become the trend of fire retardant material research and development in recent years.
Summary of the invention
Purpose of the present invention is exactly to provide a kind of good flame retardation effect, CTI value high in order to overcome the defective that above-mentioned prior art exists, and can be widely used in the antimicrobial halogen-free flame PET/PA6 alloy material in the fields such as electric, information, automobile and office equipment and preparation method thereof.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of antimicrobial halogen-free flame PET/PA6 alloy material, this alloy material is made by the component that comprises following weight part:
PET 10-30，
PA6 40-70，
Oxidation inhibitor 0.1-0.6,
Lubricant 0.1-1,
Expanding material 0.01-0.1,
Phosphorus flame retardant 5-8,
Nitrogenated flame retardant 1-8,
Antiseptic-germicide 0.2-3
Mineral powder 10-30.
The viscosity of described polyethylene terephthalate (PET) is 0.7-1.3dL/g; The viscosity of described polycaprolactam (PA6) is 2.4-2.8dL/g;
Described oxidation inhibitor is the hard ester oxidation inhibitor of tetramethylolmethane and N, and two (3, the 5-di-t-butyl-4-hydroxybenzene propionic acid amide) oxidation inhibitor of N '-hexa-methylene were by weight 1: 1 composite forming.
Described lubricant is selected from one or more in tetramethylolmethane stearate, Chinese wax oil, montanin wax;
Described expanding material is selected from one or more in two (2-oxazoline), ethylene-methyl methacrylate sodium ionomer or ethylene-methyl methacrylate zinc ionomer;
Described phosphorus flame retardant is selected from one or more mixture of triphenylphosphate, Tritolyl Phosphate, tolyl diphenyl phosphoester and polycondensation aryl phosphate ester;
Described nitrogenated flame retardant is selected from one or more the mixture in melamine cyanurate, melamine polyphosphate, melamine pyrophosphate and ammonium polyphosphate;
Described antiseptic-germicide is for carrying silver-colored zinc zeolite, and the weight content of silver is 4～8%, and the weight content of zinc is 4～8%.
Described mineral powder is through coupling agent surface-treated mica powder or talcum powder, and between 2000 orders, described coupling agent is titanate coupling agent or silane coupling agent to particle diameter at 600 orders.
A kind of preparation method of antimicrobial halogen-free flame PET/PA6 alloy material, the method comprises the following steps:
(1) get the raw materials ready according to following component and weight part content:
PET 10-30，
PA6 40-70，
Oxidation inhibitor 0.1-0.6,
Lubricant 0.1-1,
Expanding material 0.01-0.1,
Phosphorus flame retardant 5-8,
Nitrogenated flame retardant 1-8,
Antiseptic-germicide 0.2-3
Mineral powder 10-30;
(2) with polyethylene terephtalate and Poly(Trimethylene Terephthalate) PA6 respectively at 120 ℃ of lower forced air dryings 3 hours;
(3) dried PET and PA6 are mixed in high-speed mixer together with the lubricant of getting ready, oxidation inhibitor, expanding material and fire retardant, antiseptic-germicide, mineral powder;
(4) material that mixes is carried out extruding pelletization in twin screw extruder, pass through water-cooled, pelletizing, be drying to obtain product.
The temperature of the twin screw extruder described in step (4) is 200-270 ℃.
Fire retardant easily generates carbon-coating, the generation of accelerated material creepage trace under DC Electric Field.The connection that cuts off surperficial carbon granules is to improve effective means of the anti-electric trace of material.Adding of mineral powder can be played dilution fire retardant, finely dispersed effect, can effectively intercept the formation of carbon-coating under high electric field action, and can improve the Flame Retardancy energy.Mica powder, talcum powder two-dimension plane structure also have enhancement to material.Year silver-colored zinc zeolite that adds can go out silver ions, zine ion by slowly-releasing, can destroy the activity of cytolemma or the cellular plasm organized enzyme of bacterium under very low concentrations, thus killing bacteria.
Compared with prior art, the present invention has the following advantages:
1, add mineral powder can play dilution fire retardant, finely dispersed effect, can effectively intercept the formation of carbon-coating under high electric field action, and can improve the Flame Retardancy energy;
2, add mica powder, talcum powder two-dimension plane structure also the mechanical property of material to be had enhancement;
3, method is reasonable, technique is simple, non-corrosiveness γ-ray emission, safety and environmental protection.
4, good flame retardation effect, CTI value are high, can be widely used in the fields such as electric, information, automobile and office equipment.
5, year silver-colored zinc zeolite that adds can effectively be killed the bacterium of material surface.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment.
Embodiment 1
with PET and PA6 120 ℃ of lower forced air dryings 3 hours, take the PET of 30kg drying, the PA6 of 50kg drying, 0.1kg montanin wax, 0.05kg the hard ester oxidation inhibitor of tetramethylolmethane, 0.05kg N, N '-hexa-methylene two (3, 5-di-t-butyl-4-hydroxybenzene propionic acid amide), two 0.1kg (2-oxazolines), the 8kg triphenylphosphate, the 2kg melamine cyanurate, 10kg crosses the mica powder that 1200 order surfaces are processed by silane coupling agent, 0.2kg (wherein the weight content of silver is 4% to carry silver-colored zinc zeolite, the weight content of zinc is 4%) mixed 5 minutes in high-speed mixer, with the material extruding pelletization in twin screw extruder that mixes.Extruder temperature is set to: 260 ℃, 260 ℃, 255 ℃, 255 ℃, 260 ℃, 240 ℃, 220 ℃, 210 ℃, I district, II district, III district, IV district, V district, VI district, VII district, VIII district, 265 ℃ of heads, after material is extruded, through water-cooled, pelletizing, pellet was 130 ℃ of lower forced air dryings 3 hours, make batten by injection moulding machine, place after 16 hours under 23 ℃ of constant temperature and test, the performance test results sees Table 1.
Embodiment 2
with PET and PA6 120 ℃ of lower forced air dryings 3 hours, take the PET of 10kg drying, the PA6 of 70kg drying, the 1kg montanin wax, 0.3kg the hard ester oxidation inhibitor of tetramethylolmethane, 0.3kgN, N '-hexa-methylene two (3, 5-di-t-butyl-4-hydroxybenzene propionic acid amide), two 0.01kg (2-oxazolines), the 5kg triphenylphosphate, the 1kg melamine cyanurate, 14kg crosses the mica powder that 1200 order surfaces are processed by silane coupling agent, 3kg carries silver-colored zinc zeolite, and (wherein the weight content of silver is 6%, the weight content of zinc is 6%) mixed 5 minutes in high-speed mixer, with the material extruding pelletization in twin screw extruder that mixes.Extruder temperature is set to: 260 ℃, 260 ℃, 255 ℃, 255 ℃, 260 ℃, 240 ℃, 220 ℃, 210 ℃, I district, II district, III district, IV district, V district, VI district, VII district, VIII district, 265 ℃ of heads, after material is extruded, through water-cooled, pelletizing, pellet was 130 ℃ of lower forced air dryings 3 hours, make batten by injection moulding machine, place after 16 hours under 23 ℃ of constant temperature and test, the performance test results sees Table 1.
Embodiment 3
with PET and PA6 120 ℃ of lower forced air dryings 3 hours, take the PET of 14kg drying, the PA6 of 40kg drying, 0.5kg montanin wax, 0.15kg the hard ester oxidation inhibitor of tetramethylolmethane, 0.15kgN, N '-hexa-methylene two (3, 5-di-t-butyl-4-hydroxybenzene propionic acid amide), two 0.05kg (2-oxazolines), the 8kg triphenylphosphate, the 8kg melamine cyanurate, the mica powder that 30kg1200 order surface is processed by silane coupling agent, 1kg carries silver-colored zinc zeolite, and (wherein the weight content of silver is 8%, the weight content of zinc is 8%) mixed 5 minutes in high-speed mixer, with the material extruding pelletization in twin screw extruder that mixes.Extruder temperature is set to: 260 ℃, 260 ℃, 255 ℃, 255 ℃, 260 ℃, 250 ℃, 225 ℃, 200 ℃, I district, II district, III district, IV district, V district, VI district, VII district, VIII district, 260 ℃ of heads, after material is extruded, through water-cooled, pelletizing, pellet was 130 ℃ of lower forced air dryings 3 hours, make batten by injection moulding machine, place after 16 hours under 23 ℃ of constant temperature and test, the performance test results sees Table 1.
Each embodiment product performance test of table 1
Can be got by table 1 data: make through the present invention have good flame retardant resistance and high CTI value when antimicrobial halogen-free flame PET/PA6 alloy material is guaranteeing flexural strength, tensile strength and shock-resistant ability, the flame retardant resistance of excellence, and in use procedure, unharmful substance is separated out, environmental protection, efficient.
Embodiment 4
with PET and PA6 120 ℃ of lower forced air dryings 3 hours, take the PET of 14kg drying, the PA6 of 40kg drying, 0.5kg Chinese wax is oily, 0.15kg the hard ester oxidation inhibitor of tetramethylolmethane, 0.15kgN, N '-hexa-methylene two (3, 5-di-t-butyl-4-hydroxybenzene propionic acid amide), 0.05kg ethylene-methyl methacrylate sodium ionomer, the 8kg Tritolyl Phosphate, the 8kg melamine polyphosphate, the talcum powder that 30kg600 order surface is processed by silane coupling agent, 1kg carries silver-colored zinc zeolite, and (wherein the weight content of silver is 8%, the weight content of zinc is 8%) mixed 5 minutes in high-speed mixer, with the material extruding pelletization in twin screw extruder that mixes.Extruder temperature is set to: 260 ℃, 260 ℃, 255 ℃, 255 ℃, 260 ℃, 250 ℃, 225 ℃, 200 ℃, I district, II district, III district, IV district, V district, VI district, VII district, VIII district, 270 ℃ of heads, after material is extruded, through water-cooled, pelletizing, pellet was 130 ℃ of lower forced air dryings 3 hours, make batten by injection moulding machine, place after 16 hours under 23 ℃ of constant temperature and test, the performance test results sees Table 1.
Embodiment 5
with PET and PA6 120 ℃ of lower forced air dryings 3 hours, take the PET of 14kg drying, the PA6 of 40kg drying, 0.5kg tetramethylolmethane stearate, 0.15kg the hard ester oxidation inhibitor of tetramethylolmethane, 0.15kgN, N '-hexa-methylene two (3, 5-di-t-butyl-4-hydroxybenzene propionic acid amide), 0.05kg ethylene-methyl methacrylate zinc ionomer, 4kg tolyl diphenyl phosphoester, 4kg polycondensation aryl phosphate ester, the 4kg melamine pyrophosphate, the 4kg ammonium polyphosphate, the talcum powder that 30kg2000 order surface is processed by silane coupling agent, 1kg carries silver-colored zinc zeolite, and (wherein the weight content of silver is 8%, the weight content of zinc is 8%) mixed 5 minutes in high-speed mixer, with the material extruding pelletization in twin screw extruder that mixes.Extruder temperature is set to: 260 ℃, 260 ℃, 255 ℃, 255 ℃, 260 ℃, 250 ℃, 225 ℃, 200 ℃, I district, II district, III district, IV district, V district, VI district, VII district, VIII district, 270 ℃ of heads, after material is extruded, through water-cooled, pelletizing, pellet was 130 ℃ of lower forced air dryings 3 hours, make batten by injection moulding machine, place after 16 hours under 23 ℃ of constant temperature and test, the performance test results sees Table 1.
Above disclosed be only several specific embodiments of the application, but the application is not limited thereto, the changes that any person skilled in the art can think of all should drop in the application's protection domain.
Claims (10)
1. an antimicrobial halogen-free flame PET/PA6 alloy material, is characterized in that, this alloy material is made by the component that comprises following weight part:
PET 10-30，
PA6 40-70，
Oxidation inhibitor 0.1-0.6,
Lubricant 0.1-1,
Expanding material 0.01-0.1,
Phosphorus flame retardant 5-8,
Nitrogenated flame retardant 1-8,
Antiseptic-germicide 0.2-3,
Mineral powder 10-30.
2. a kind of antimicrobial halogen-free flame PET/PA6 alloy material according to claim 1, is characterized in that, the viscosity of described PET is 0.7-1.3dL/g; The viscosity of described PA6 is 2.4-2.8dL/g.
3. a kind of antimicrobial halogen-free flame PET/PA6 alloy material according to claim 1, it is characterized in that, described oxidation inhibitor is the hard ester oxidation inhibitor of tetramethylolmethane and N, and two (3, the 5-di-t-butyl-4-hydroxybenzene propionic acid amide) oxidation inhibitor of N '-hexa-methylene were by weight 1: 1 composite forming.
4. a kind of antimicrobial halogen-free flame PET/PA6 alloy material according to claim 1, is characterized in that, described lubricant is selected from one or more in tetramethylolmethane stearate, Chinese wax oil and montanin wax.
5. a kind of antimicrobial halogen-free flame PET/PA6 alloy material according to claim 1, it is characterized in that, described expanding material is selected from one or more in two (2-oxazoline), ethylene-methyl methacrylate sodium ionomer or ethylene-methyl methacrylate zinc ionomer.
6. a kind of antimicrobial halogen-free flame PET/PA6 alloy material according to claim 1, it is characterized in that, described phosphorus flame retardant is selected from one or more the mixture in triphenylphosphate, Tritolyl Phosphate, tolyl diphenyl phosphoester and polycondensation aryl phosphate ester.
7. a kind of antimicrobial halogen-free flame PET/PA6 alloy material according to claim 1, it is characterized in that, described nitrogenated flame retardant is selected from one or more the mixture in melamine cyanurate, melamine polyphosphate, melamine pyrophosphate and ammonium polyphosphate.
8. a kind of antimicrobial halogen-free flame PET/PA6 alloy material according to claim 1, is characterized in that, described antiseptic-germicide is for carrying silver-colored zinc zeolite, and the weight content of silver is 4～8%, and the weight content of zinc is 4～8%.
9. a kind of antimicrobial halogen-free flame PET/PA6 alloy material according to claim 1, it is characterized in that, described mineral powder is through coupling agent surface-treated mica powder or talcum powder, and between 2000 orders, described coupling agent is titanate coupling agent or silane coupling agent to particle diameter at 600 orders.
10. the preparation method of an antimicrobial halogen-free flame PET/PA6 alloy material as claimed in claim 1, is characterized in that, the method comprises the following steps:
(1) get the raw materials ready according to following component and weight part content:
PET 10-30，
PA6 40-70，
Oxidation inhibitor 0.1-0.6,
Lubricant 0.1-1,
Expanding material 0.01-0.1,
Phosphorus flame retardant 5-8,
Nitrogenated flame retardant 1-8,
Antiseptic-germicide 0.2-3,
Mineral powder 10-30;
(2) PET and PA6 were respectively at 120 ℃ of lower forced air dryings 3 hours;
(3) dried PET and PA6 are mixed in high-speed mixer together with the lubricant of getting ready, oxidation inhibitor, expanding material and fire retardant, antiseptic-germicide, mineral powder;
(4) material that mixes is carried out extruding pelletization in twin screw extruder, pass through water-cooled, pelletizing, be drying to obtain product; The temperature of described twin screw extruder is 200-270 ℃.
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| CN105400158A (en) * | 2015-12-16 | 2016-03-16 | 华南理工大学 | Reinforced flame-retardation PBT/PA6 composite material and preparation method thereof |
| CN105419317A (en) * | 2015-12-25 | 2016-03-23 | 南宁学院 | Novel nylon 6-polybutylene terephthalate flame retardant alloy material and preparation method thereof |
| CN112341779A (en) * | 2020-10-21 | 2021-02-09 | 工业和信息化部电子第五研究所华东分所 | High CTI halogen-free flame-retardant reinforced polycarbonate and preparation method and application thereof |
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| CN112341779A (en) * | 2020-10-21 | 2021-02-09 | 工业和信息化部电子第五研究所华东分所 | High CTI halogen-free flame-retardant reinforced polycarbonate and preparation method and application thereof |
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