CN103013104A - Halogen-free filling flame-retardant nylon 6 composite material and preparation method thereof - Google Patents
Halogen-free filling flame-retardant nylon 6 composite material and preparation method thereof Download PDFInfo
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- CN103013104A CN103013104A CN2012105760986A CN201210576098A CN103013104A CN 103013104 A CN103013104 A CN 103013104A CN 2012105760986 A CN2012105760986 A CN 2012105760986A CN 201210576098 A CN201210576098 A CN 201210576098A CN 103013104 A CN103013104 A CN 103013104A
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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
- B29C48/04—Particle-shaped
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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
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
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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
- B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
- B29C48/875—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
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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
-
- 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
-
- 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
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
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- Engineering & Computer Science (AREA)
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- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
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Abstract
The invention provides a halogen-free filling flame-retardant nylon 6 composite material and a preparation method thereof. The halogen-free filling flame-retardant nylon 6 composite material provided by the invention is characterized by being prepared from the following raw materials: 53-70 parts by weight of nylon 6 resin, 7-15 parts by weight of melamine cyanurate, 20-30 parts by weight of inorganic filling material, 0-5 parts by weight of synergistic flame retardant, and 1-5 parts by weight of processing agent. Compared with the prior art, the halogen-free filling flame-retardant nylon 6 composite material provided by the invention has the beneficial effects the halogen-free filling flame-retardant nylon 6 composite material is capable of passing the GWFI (Glow Wire Flammability Index) test at 960 DEG C, also has the characteristics of being low in cost, high in modulus and strength, excellent size stability, environment-friendly, flame-retardant and the like, and has good application prospect.
Description
Technical field
The present invention relates to high molecular fire retardant material preparation method field, particularly Halogen is filled flame-retardant nylon 6 material and preparation method thereof.
Background technology
Along with the development of electronic enterprises, the demand of fire-retardant nylon material keeps rapid growth.Although the halogen containing flame-retardant good flame retardation effect, the amount of being fuming is large during burning, and the generation toxic gas causes secondary pollution.Melamine cyanurate is called for short MCA, is a kind of nitrogenous compound that trimeric cyanamide and cyanuric acid are polymerized.As a kind of nitrogenated flame retardant, to compare with halogenated flame retardant, toxicity is lower, has excellent flame-retardant comprehensive performance.Nylon 6 is that a kind of toughness is good, electrical property excellence, oil resistant, wear-resisting important engineering plastics, but it also needs to carry out fire-retardant finish when being applied to electronic apparatus, transportation building field.
" polymer material science and engineering " 20 (3) phases, Chinese patent 200510022046.4, Chinese patent 03135668.0 in 2004 discloses trimeric-cyanamide cyanurate fire-retardant nylon.But a kind of mode of above research is that melamine cyanurate is carried out molecule is composite modified, then prepares fire-retardant nylon, and another kind of mode is to prepare first fire retardant with the original position complex method.Chinese patent 200710011841.2 provides a kind of mixes nylon 6, melamine cyanurate, oxidation inhibitor, triphenylphosphate or zinc borate, adopt the reaction extrusion method to prepare melamine cyanurate/nylon 6 fire retardant materials, flame retardant properties can reach UL94V-0, but and the data such as unexposed GWFI test and mechanical property.
JP 60037829B2 has described a kind of flame-retardant polyamide composition, weight based on polymeric amide, comprise the melamine cyanurate of 3-30 % by weight and the mineral filler of 5-60 % by weight (for example talcum powder), wherein the weight ratio of melamine cyanurate/mineral filler is adjusted between 1/5 and 1/3, illustrational composition all contain the mineral filler of 30wt% and the melamine cyanurate of 10wt% (this corresponding to based on the mineral filler of the total amount 21.4wt% of composition and the melamine cyanurate of 7.1wt%) based on the weight of polymeric amide.The shortcoming of this known daiamid composition is that the amount of filler is restricted.
Chinese patent application 200980126940.2, flame-retardant polyamide composition, a kind of daiamid composition is disclosed, said composition comprises polymeric amide, melamine cyanurate and as the talcum of mineral filler, wherein the amount of talcum is higher than 25wt%, and the weight ratio of melamine cyanurate/talcum is higher than 1/3.When the talcous content that is used for daiamid composition is 25%, increase the consumption of MAC, do not make the shortening of combustion time; When the amount of used talcum surpassed 25%, the consumption of increase MAC to the weight ratio of poly cyanamid cyanurate/talcum was higher than at 1/3 o'clock, can cause shorten combustion time, passes through smoothly the test of 960 ℃ of glowing filaments.Said composition is generally used for the electrical and electronic parts industry, is mainly used in for miniature circuit breaker.
There are the problems such as non-environmental protection flame retardant, flame retardant rating is low, the GWFI test is unstable in existing fire-retardant filled nylon.Therefore, invent a kind of daiamid composition that possesses the characteristics such as GWFI stable testing, environmental protection flame retardant, possess good application prospect at the Low-voltage Electronic appliance field.
Summary of the invention
The purpose of this invention is to provide and a kind ofly fill the fire-retardant Nylon 6 matrix material with the fire-retardant Halogen of Inorganic Fillers Filled, melamine cyanurate and synergistic fire retardant, be applicable to the Low-voltage Electronic electric equipment products.Refer to the GWFI test under passing through 960 ℃ smoothly acceptable combustion time of the present invention.
In order to achieve the above object, the invention provides a kind of Halogen and fill the fire-retardant Nylon 6 matrix material, it is characterized in that, made by following raw material:
Nylon 6 53-70 weight part;
Melamine cyanurate 7-15 weight part;
Mineral filler 20-30 weight part;
Synergistic fire retardant 0-5 weight part;
Processing aid 1-5 weight part;
Described mineral filler is the one or more kinds of mixtures in talcum powder, wollastonite, globular glass microballon and the flat glass fiber.
Described Nylon 6 is preferably the low viscosity Nylon 6, and more preferably relative viscosity is the Nylon 6 of 2.2-2.5.
Preferably, described talcous median size is the 1000-5000 order; The length-to-diameter ratio of described wollastonite is 10-20: 1; The diameter of described globular glass microballon is 10-30 μ m; The dimensional ratios that described flat glass fiber is preferably main cross section axle and time cross section axis is 2-6, and length is the chopped flat glass fiber of 2-3mm.
Described synergistic fire retardant is preferably the one or more kinds of mixtures in zinc borate, phosphonium flame retardant and the polynite.
More preferably, described phosphonium flame retardant is a kind of or its mixture in phenoxy phosphazene compound and the triphenylphosphate.Described polynite is that average wafer thickness is less than the sodium-based montmorillonite of 25nm.
Described processing aid is preferably at least a in lubricant, oxidation inhibitor, stablizer and the releasing agent.
More preferably, described lubricant is one or more the composition in fatty acid ester blends, white mineral oil and the pentaerythritol stearate; Described oxidation inhibitor is a kind of or its composition in Hinered phenols antioxidant and the phosphite ester kind antioxidant; Described releasing agent is stearate; Described stablizer is the aromatic amine stablizer.
Further; described Hinered phenols antioxidant is that four (methylene radical-3-(3; the 5-di-tert-butyl-hydroxy phenyl) propionic ester) methane, N; [3-(3 for N '-two; the 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine, triglycol two-3-(3-tertiary butyl-4-hydroxy-5-aminomethyl phenyl) propionic ester, β-(4-hydroxyl-3; the 5-di-tert-butyl-phenyl) the positive octadecanol ester of propionic acid or N, N '-two [3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl] hydrazine.
Further, described phosphorous acid esters antioxidant is three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester, two (2.4-di-tert-butyl-phenyl) pentaerythritol diphosphites, four (2, the 4-di-tert-butylphenol)-4,4 '-xenyl diphosphites or two (2,6-di-tert-butyl-phenyl) pentaerythritol diphosphites or triphenyl phosphite.
The present invention also provides above-mentioned Halogen to fill fire-retardant Nylon 6 composite manufacture method, it is characterized in that concrete steps are:
The first step: Nylon 6 53-70 weight part, melamine cyanurate 7-15 weight part, mineral filler 20-30 weight part, synergistic fire retardant 0-5 weight part and processing aid 1-5 weight part are added high mixer be mixed to get Preblend;
Second step: the Preblend that the first step is obtained joins the twin screw extruder from the main spout of twin screw extruder, melt extrudes, cooling granulation, obtains Halogen and fills the fire-retardant Nylon 6 matrix material, wherein, the processing parameter of twin screw extruder is: 210 ℃ of district's temperature, 230 ℃ of two district's temperature, 250 ℃ of three district's temperature, 250 ℃ of four district's temperature, 240 ℃ of five district's temperature, 240 ℃ of six district's temperature, 240 ℃ of seven district's temperature, 230 ℃ of eight district's temperature, 240 ℃ of nine district's temperature; 350 rev/mins of engine speeds.
Halogen of the present invention is filled the fire-retardant Nylon 6 matrix material mainly for the manufacture of the low-voltage apparatus goods.
Compared with prior art, the invention has the beneficial effects as follows:
Halogen of the present invention is filled the fire-retardant Nylon 6 matrix material can be by 960 ℃ of lower GWFI tests, also possess the characteristics such as dimensional stability, environmental protection flame retardant of low cost, high-modulus, high strength and excellence, possess good application prospect.
Compare with background technology " polymer material science and engineering " 20 (3) phases, Chinese patent 200510022046.4, Chinese patent 03135668.0 in 2004, it is composite modified that the present invention does not carry out molecule to melamine cyanurate, then prepares fire-retardant nylon; Neither prepare first fire retardant at modification of nylon with the original position complex method, but directly melt extrude modification of nylon with the melamine cyanurate process, preparation technology of the present invention is more simple by contrast, and Production Flow Chart and cycle are short, save cost.Compare with Chinese patent 200710011841.2, JP 60037829B2 and Chinese patent application 200980126940.2, the present invention keeps the material excellent mechanical performances by adding mineral filler (comprising talcum powder, wollastonite, glass microballon, flat glass) in the flame retardant properties that improves material, this is because the adding of these mineral fillers improves the performances such as modulus of material by enhancement; Be on the other hand, during burning in the expansion process of carburization zone, mineral filler can well combine with carburization zone, be conducive to the formation of finer and close carburization zone or can effectively strengthen resin matrix and carburization zone, a part that so just can be used as carburization zone strengthens flame retardant properties, has so just significantly improved flame retardant resistance.The simultaneously selection of synergistic fire retardant and with filler be used Flame Retardancy can and the raising of mechanical property aspect playing very crucial effect.
Embodiment
For the present invention is become apparent, hereby with preferred embodiment, be described in detail below.
Embodiment 1-11
In the raw material that embodiment 1-11 adopts, nylon 6 is PA6M2400 (newly understand U.S.A and reach production); Melamine cyanurate is commercially available powder (production of Sichuan fine chemistry industry); Talcum powder is 3000 purpose superfine talcum powders; Wollastonite is that length-to-diameter ratio is 15-20: 1 needle-like wollastonite; The mean diameter of globular glass microballon is about 15 μ m; Flat glass fiber is that the dimensional ratios of main cross section axle and time cross section axis is 2, and length is the chopped strand of 2-3mm.Polynite is the sodium-based montmorillonite DK5 of Zhejiang Feng Hong clay Chemical Manufacture; Zinc borate is the ZB-2335 of Zibo rising sun shellfish Chemical Manufacture; The phenoxy group polyphosphonitrile is the KP-735NA of Zibo blue seal Chemical Manufacture; Triphenylphosphate is that Anhua worker of Changzhou section produces; Stablizer is polycarbodiimide, adopts the STABAXOL-1 of TUV chemical production; Oxidation inhibitor is N, N '-two-(3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (Irganox 1098 of Ciba company) and three [2.4-di-tert-butyl-phenyl] phosphorous acid ester (Irganox 168 of Ciba company); Lubricant is the TR044 of U.S. Struktol company; Releasing agent is calcium stearate.
The weight part proportioning of each raw material is according to shown in the table 1 in embodiment 1-11 and the Comparative Examples, and its preparation method is as follows:
(1) according to each material content (weight part) each raw material is added high mixer and be mixed to get Preblend;
(2) the main spout of Preblend from twin screw extruder joined the twin screw extruder, melt extrude, cooling granulation, obtain Halogen and fill the fire-retardant Nylon 6 matrix material, wherein, the processing parameter of twin screw extruder is: 210 ℃ of district's temperature, 230 ℃ of two district's temperature, 250 ℃ of three district's temperature, 250 ℃ of four district's temperature, 240 ℃ of five district's temperature, 240 ℃ of six district's temperature, 240 ℃ of seven district's temperature, 230 ℃ of eight district's temperature, 240 ℃ of nine district's temperature; 350 rev/mins of engine speeds.
Method for testing performance of the present invention and standard are:
Tensile strength is tested according to the ISO527-2 standard; Flexural strength and modulus in flexure are tested according to the ISO178 standard; Notched Izod impact strength is tested according to the ISO179 standard; Fire-retardant GWFI test is according to the IEC60695 standard testing, and each test result is as shown in table 1.
As can be seen from Table 1, Halogen prepared in accordance with the present invention is filled the fire-retardant Nylon 6 matrix material and is not only had good mechanical property, and has an excellent flame retardant properties, can be widely used in Low-voltage Electronic electrical equipment, etc. field that material mechanical performance and flame retardant properties are had relatively high expectations, fully satisfy the GWFI test request.The present invention is by the flame-retardant nylon 6 material of MCA or MCA and synergistic fire retardant, can be smoothly by 960 ℃, the GWFI testing level of 1mm, during burning, low cigarette, low toxicity keep the modulus of good mechanical property, especially material to significantly improve simultaneously on the material monolithic, and the good fluidity of system, be beneficial to process for processing.Compare with other flame-retardant nylon 6 materials, fire retardant material of the present invention is the fire retardant material of efficient halogen-free environmental protection, can fully satisfy the low-voltage apparatus service requirements.
Claims (7)
1. a Halogen is filled the fire-retardant Nylon 6 matrix material, it is characterized in that, is made by following raw material:
Nylon 6 53-70 weight part;
Melamine cyanurate 7-15 weight part;
Mineral filler 20-30 weight part;
Synergistic fire retardant 0-5 weight part;
Processing aid 1-5 weight part;
Described mineral filler is the one or more kinds of mixtures in talcum powder, wollastonite, globular glass microballon and the flat glass fiber.
2. Halogen as claimed in claim 1 is filled the fire-retardant Nylon 6 matrix material, it is characterized in that described Nylon 6 is that relative viscosity is the Nylon 6 of 2.2-2.5.
3. Halogen as claimed in claim 1 is filled the fire-retardant Nylon 6 matrix material, it is characterized in that described synergistic fire retardant is the one or more kinds of mixtures in zinc borate, phosphonium flame retardant and the polynite.
4. Halogen as claimed in claim 3 is filled the fire-retardant Nylon 6 matrix material, it is characterized in that described phosphonium flame retardant is a kind of or its mixture in phenoxy phosphazene compound and the triphenylphosphate.
5. Halogen as claimed in claim 1 is filled the fire-retardant Nylon 6 matrix material, it is characterized in that, described processing aid is at least a in lubricant, oxidation inhibitor, stablizer and the releasing agent.
6. Halogen as claimed in claim 5 is filled the fire-retardant Nylon 6 matrix material, it is characterized in that, described lubricant is one or more the composition in fatty acid ester blends, white mineral oil and the pentaerythritol stearate; Described oxidation inhibitor is a kind of or its composition in Hinered phenols antioxidant and the phosphite ester kind antioxidant; Described releasing agent is stearate; Described stablizer is the aromatic amine stablizer.
7. Halogen claimed in claim 1 is filled fire-retardant Nylon 6 composite manufacture method, it is characterized in that concrete steps are:
The first step: Nylon 6 53-70 weight part, melamine cyanurate 7-15 weight part, mineral filler 20-30 weight part, synergistic fire retardant 0-5 weight part and processing aid 1-5 weight part are added high mixer be mixed to get Preblend;
Second step: the Preblend that the first step is obtained joins the twin screw extruder from the main spout of twin screw extruder, melt extrudes, cooling granulation, obtains Halogen and fills the fire-retardant Nylon 6 matrix material, wherein, the processing parameter of twin screw extruder is: 210 ℃ of district's temperature, 230 ℃ of two district's temperature, 250 ℃ of three district's temperature, 250 ℃ of four district's temperature, 240 ℃ of five district's temperature, 240 ℃ of six district's temperature, 240 ℃ of seven district's temperature, 230 ℃ of eight district's temperature, 240 ℃ of nine district's temperature; 350 rev/mins of engine speeds.
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| CN201210576098.6A CN103013104B (en) | 2012-12-26 | 2012-12-26 | Halogen-free filling flame-retardant nylon 6 composite material and preparation method thereof |
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Cited By (26)
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| CN103910999A (en) * | 2014-04-02 | 2014-07-09 | 合肥杰事杰新材料股份有限公司 | High-glowing nylon 6 composition and preparation method thereof |
| DE202014008607U1 (en) | 2014-10-31 | 2014-11-24 | Lanxess Deutschland Gmbh | polyamide compositions |
| CN104292818A (en) * | 2014-09-09 | 2015-01-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Method of nano halogen-free flame retardant polyamide-6 |
| EP2924069A1 (en) | 2014-03-26 | 2015-09-30 | LANXESS Deutschland GmbH | Polyamide compositions |
| EP2924065A1 (en) * | 2014-03-26 | 2015-09-30 | LANXESS Deutschland GmbH | Polyamide compositions |
| CN104945896A (en) * | 2014-03-26 | 2015-09-30 | 朗盛德国有限责任公司 | Polyamide composition |
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| CN107987524A (en) * | 2017-12-11 | 2018-05-04 | 青岛科技大学 | A kind of preparation of low-cost and high-performance halogen-free flame-retardant nylon material |
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| CN112041382A (en) * | 2018-04-13 | 2020-12-04 | 巴斯夫欧洲公司 | Flame-retardant thermoplastic molding compositions |
| CN112778757A (en) * | 2020-12-28 | 2021-05-11 | 金发科技股份有限公司 | High-density nylon composite material and preparation method and application thereof |
| CN115433456A (en) * | 2022-09-14 | 2022-12-06 | 广东聚石化学股份有限公司 | High-flame-retardant and high-impact-resistant melamine cyanurate flame-retardant nylon composition as well as preparation method and application thereof |
| CN115637042A (en) * | 2022-11-04 | 2023-01-24 | 杭州明日新材料科技有限公司 | Nitrogen-series flame-retardant nylon modified material with high glowing filament ignition temperature |
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