CN101565543A - Halogen-free flame-retardant nylon 6 material and preparation method thereof - Google Patents
Halogen-free flame-retardant nylon 6 material and preparation method thereof Download PDFInfo
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- CN101565543A CN101565543A CNA2009100315848A CN200910031584A CN101565543A CN 101565543 A CN101565543 A CN 101565543A CN A2009100315848 A CNA2009100315848 A CN A2009100315848A CN 200910031584 A CN200910031584 A CN 200910031584A CN 101565543 A CN101565543 A CN 101565543A
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Abstract
The invention discloses a halogen-free flame-retardant nylon 6 material and a preparation method thereof, which belong to the technical field of polymer materials. The material is prepared from the following raw materials: a nylon 6 raw material, a heat stabilizer, an antioxidant, a halogen-free flame retardant, a processing modifier, an inorganic powder filler, fiberglass and pigment. The preparation method comprises the following steps of measuring the raw materials, mixing various raw materials fully and evenly through a high-mixing machine, and preparing a nylon 6 major material; and extruding the nylon 6 major material through an extruder for granulation and forming the halogen-free flame-retardant nylon 6 material. The halogen-free flame-retardant nylon 6 material has the advantages of good mechanical properties, flame retardancy, high-temperature resistance, capability of being widely applied to electrical-appliance components, control switches, rotary switch timers and the like, and better flame-retardant effect compared with the prior halogen-containing flame retardant, as well as no carcinogenic substances in production process and final products.
Description
Technical field
The present invention relates to technical field of polymer materials, specifically is a kind of halogen-free flame-retardant nylon 6 material and preparation method thereof.
Background technology
Traditional halogen containing flame-retardant can make material obtain good flame-retardant effect, but owing to discharge a large amount of smog and hydrogen halide stimulation eyes and respiratory system, can cause " secondary disaster ".Particularly many bromines hexichol class (PBDB) and polybromodiphenyl ether class (PBDBE), can produce two English class materials, may cause that human body metabolism is not normal and cause symptom such as anxiety, insomnia, headache, eye illness, arteriosclerosis, liver neoplasm that the experimentation on animals discovery can cause cancer.On the other hand, it is also quite difficult to handle or reclaim these Halogen waste materials, so the use of halogen containing flame-retardant has been subjected to considerable restraint.The halogen-free flame retardants of nylon 6 usefulness mainly contains trimeric cyanamide (MA), MA derivative (compound system that comprises them), phosphorus flame retardant and metal hydroxides, red phosphorus, ammonium polyphosphate (APP).
Summary of the invention
For overcoming the above-mentioned deficiency of prior art, the invention provides a kind of halogen-free flame-retardant nylon 6 material and preparation method thereof.Can reduce cost, can satisfy its outward appearance and internal performance requirement simultaneously again.Than the good flame retardation effect of traditional halogen containing flame-retardant, and production process and the finished product do not have carcinogenic substance.
The present invention is achieved through the following technical solutions: a kind of halogen-free flame-retardant nylon 6 material, to form by following main ingredient, and the weight part of each component is:
6 50～70 parts of nylon;
10～50 parts of mineral filler or glasses;
0.2～0.7 part of stablizer;
0.5～1 part of modifier;
0.1～0.5 part in oxidation inhibitor;
10～20 parts of halogen-free flame retardantss.
Can also add pigment in the described formation halogen-free flame-retardant nylon 6 material, the consumption of pigment adds according to the requirement to color.
Described mineral filler is that described mineral filler is water-ground limestone, light calcium carbonate, kaolin, talcum powder, silicon-dioxide, magnesium hydroxide, aluminium hydroxide or wollastonite, and above-mentioned substance is by the mixture of making a gesture of measuring combination arbitrarily; Glass is general roving glass fiber in market or short glass fiber.Described thermo-stabilizer is that cuprous iodide, potassiumiodide, Zinic stearas or above-mentioned substance are by the mixture of making a gesture of measuring arbitrarily.
Described modifier is calcium stearate, ethylene bis stearamide or surface-modifying agent TAF class material.
Described oxidation inhibitor is N, N '-1,6-hexylidene-two-[3,5-di-t-butyl-4-hydroxybenzene propionic acid amide], three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester, four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid stearyl alcohol ester and composition thereof.
Described halogen-free flame retardants is nitrogen system, nitrogen phosphorus system, phosphorus system, and the arbitrary combination mixture of above-mentioned substance.
A kind of preparation method of halogen-free flame-retardant nylon 6 material is characterized in that: its preparation method may further comprise the steps:
(1) major ingredient of preparation halogen-free flame-retardant nylon 6 material:
Nylon 6 pellets are put into high mixer, then thermo-stabilizer, oxidation inhibitor are put into high mixer, mix and stirred 2-5 minute, again mineral filler powder, modifier, pigment are put into high mixer and continued to mix stirring 2-5 minute, add halogen-free flame retardants mixing discharging after 2-5 minute at last, the material of emitting is the major ingredient of halogen-free flame-retardant nylon 6 material.
(2) preparation halogen-free flame-retardant nylon 6 material:
Major ingredient extruding pelletization on twin screw extruder with halogen-free flame-retardant nylon 6 material, one district's temperature is 220～250 ℃ from the spout to the die head, 225～250 ℃ of two district's temperature, 230～240 ℃ of three district's temperature, 235～250 ℃ of four district's temperature, 235～250 ℃ of five district's temperature, 220～240 ℃ of six district's temperature, 235～255 ℃ of seven district's temperature, 235～255 ℃ of eight district's temperature, 250 ℃ of head temperatures; Residence time is 0.5～2min, and engine speed is 200～440r/min, and pressure is 10～15MPa, discharging, extrudes postcooling, drying, pelletizing, the halogen-free flame-retardant nylon 6 material finished product.
The invention has the beneficial effects as follows:
1. add the mineral filler powder in this halogen-free flame-retardant nylon 6 material, can be according to practical situation, under the prerequisite that does not reduce performance index, select for use different additions and kind mineral filler powder to reach the purpose that reduces production costs, can reduce by 5%～15% cost than traditional halogen-containing product comparison, improve competition capability effectively.The halogen-free flame-retardant nylon 6 material thermostability obtains bigger raising.
With mould Dai Gang, to mould Dai Mu, reach the social benefit of saving resource; Light specific gravity is 1/7 of steel approximately; Dimensional stability is good; Have favorable mechanical performance and processing characteristics; Ageing-resistant, corrosion-resistant; Electrical insulating property is good, and is nontoxic, odorless, good weatherability; Has excellent high-temperature stability;
3. traditional halogen containing flame-retardant is many bromines hexichol class (PBDB) and polybromodiphenyl ether class (PBDBE) particularly, can produce two mouthfuls and dislike English class material, may cause that human body metabolism is not normal and cause symptom such as anxiety, insomnia, headache, eye illness, arteriosclerosis, liver neoplasm that the experimentation on animals discovery can cause cancer; This product then can not produce the material that makes the carcinogenic disease of people.
Embodiment
The present invention is described in further detail by following examples, but following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Embodiment 1
The halogen-free flame-retardant nylon 6 material composition of raw materials:
Nylon 6 75kg
Roving glass fiber 45kg
Zinic stearas 450g
Ethylene bis stearamide 750g
Four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 450g
Three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester 300g
Nitrogen flame retardant 30kg.
Nylon 6 pellets are put into high mixer, then with thermo-stabilizer, four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester is put into high mixer, mix and stirred 2～5 minutes, ethylene bis stearamide is put into high mixer again and continued and mix stirring 2～5 minutes, add the nitrogen flame retardant at last and mix discharging after 2～5 minutes, the material of emitting is the major ingredient of halogen-free flame-retardant nylon 6 material;
The powder of the halogen-free flame-retardant nylon 6 material of producing by this prescription promptly can be made into halogen-free flame-retardant nylon 6 material through extrusion shaping machine (parallel parallel dual-screw extruding machine) extruding pelletization.The manufacturing process of halogen-free flame-retardant nylon 6 material is:
| One district | Two districts | Three districts | Four districts | Five districts | Six districts | Seven districts | Eight districts | Head | |
| Temperature/℃ | 225～ 230 | 225～ 230 | 230～ 235 | 230～ 235 | 235～ 240 | 235～ 240 | 240～ 245 | 240～ 245 | 250 |
Residence time is 0.5～2min, and engine speed is 400r/min, and pressure is 10～15MPa, discharging, extrudes postcooling, drying, pelletizing, the halogen-free flame-retardant nylon 6 material finished product.
Embodiment 2
The halogen-free flame-retardant nylon 6 material composition of raw materials:
Nylon 6 87kg
Roving glass fiber 45kg
Zinic stearas 450g
Ethylene bis stearamide 750g
Four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 450g
Three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester 300g
Halogen-free flame retardants 18kg
Black Masterbatch 1.5kg.
Nylon 6 pellets are put into high mixer, then with thermo-stabilizer, four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester is put into high mixer, mix and stirred 2～5 minutes, ethylene bis stearamide, black Masterbatch are put into high mixer again and continued and mix stirring 2～5 minutes, add phosphorus flame retardant at last and mix discharging after 2～5 minutes, the material of emitting is the major ingredient of halogen-free flame-retardant nylon 6 material;
With the major ingredient of the halogen-free flame-retardant nylon 6 material of above-mentioned preparation, extruding pelletization on twin screw extruder, halogen-free flameproof PA6 finished product.Extruding and pelletizing process (temperature ℃) parameter is identical with embodiment 1.
Embodiment 3
The halogen-free flame-retardant nylon 6 material composition of raw materials:
Nylon 6 90kg
Roving glass fiber 30kg
Zinic stearas 450g
Calcium stearate 750g
N, N '-hexamethylene-two-[3,5-di-t-butyl-4-hydroxybenzene propionic acid amide] 450g
Four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 300g
Nitrogen flame retardant 30kg.
Nylon 6 pellets are put into high mixer, then with thermo-stabilizer, four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester is put into high mixer, mix and stirred 2～5 minutes, ethylene bis stearamide is put into high mixer again and continued and mix stirring 2～5 minutes, add the nitrogen flame retardant at last and mix discharging after 2～5 minutes, the material of emitting is the major ingredient of halogen-free flame-retardant nylon 6 material;
With the major ingredient of the halogen-free flame-retardant nylon 6 material of above-mentioned preparation, extruding pelletization on twin screw extruder, halogen-free flameproof PA6 finished product.Extruding and pelletizing process (temperature ℃) parameter is identical with embodiment 1.
Above examples of implementation can be according to practical situation, the purpose of selecting for use the inorganic mineral filler of different additions or glass to also have halogen-free flame retardants to reach under the prerequisite that reaches the performance that designing institute needs to reduce production costs can be saved 5%～15% cost according to different additions and corresponding common product comparison.
The made product of embodiment is detected by Tianjin quality monitoring testing station the 5th station, reaches corresponding national standards fully.
Compare with halogenated flame retardant, phosphorus flame retardant toxicity, living cigarette and corrodibility are all lower.Phosphorus flame retardant can use separately, also can wait other fire retardants to be used with nitrogen system, produces synergistic effect.In gas phase, phosphorus flame retardant plays fire retardation by catching O or HO free radical.In addition, phosphorus flame retardant also can be taken away heat by impelling some superpolymer accelerated degradation drippage; The water of deviating from simultaneously volatilization makes the combustion substance cooling and slows down or stop thermal destruction thereby the time also can absorb a large amount of heat; And form the concentration that water vapour has diluted flammable volatile matter and oxygen at flame zone, so phosphorus flame retardant has multiple anti-flaming function.Nitrogen flame retardant low toxicity, burn into is not good and inexpensive to heat and UV stable, flame retarding efficiency.Shortcoming is with its fire-retardant plastic working difficulty, and is dispersed relatively poor in base material.The nitrogen flame retardant that is applicable to nylon 6 mainly contains MCA (trimeric cyanamide-cyanurate), melamine (trimeric cyanamide), melamine phosphate etc.Pyrolysis takes place when the nitrogen flame retardant is heated, and principal product is NH
3, H
2NCN, N
2, NO, NO
2, CO
2, H
2Non-flammable gases such as O.
Claims (8)
1. halogen-free flame-retardant nylon 6 material, it is characterized in that: be made up of following main ingredient, the weight part of each component is:
650～70 parts of nylon;
10～50 parts of mineral filler or glasses;
0.2～0.7 part of stablizer;
0.5～1 part of modifier;
0.1～0.5 part in oxidation inhibitor;
10～20 parts of halogen-free flame retardantss.
2. halogen-free flame-retardant nylon 6 material according to claim 1 is characterized in that: can also add pigment in the described formation halogen-free flame-retardant nylon 6 material, the consumption of pigment adds according to the requirement to color.
3. halogen-free flame-retardant nylon 6 material according to claim 1, it is characterized in that: described mineral filler is water-ground limestone, light calcium carbonate, kaolin, talcum powder, silicon-dioxide, magnesium hydroxide, aluminium hydroxide or wollastonite, and above-mentioned substance is by the mixture of making a gesture of measuring combination arbitrarily; Glass is general roving glass fiber in market or short glass fiber.
4. halogen-free flame-retardant nylon 6 material according to claim 1 is characterized in that: described thermo-stabilizer is that cuprous iodide, potassiumiodide, Zinic stearas or above-mentioned substance are by the mixture of making a gesture of measuring arbitrarily.
5. halogen-free flame-retardant nylon 6 material according to claim 1 is characterized in that: described modifier is calcium stearate, ethylene bis stearamide or surface-modifying agent TAF class material.
6. halogen-free flame-retardant nylon 6 material according to claim 1, it is characterized in that: described oxidation inhibitor is N, N '-1,6-hexylidene-two-[3,5-di-t-butyl-4-hydroxybenzene propionic acid amide], three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester, four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester or β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid stearyl alcohol ester and composition thereof.
7. halogen-free flame-retardant nylon 6 material according to claim 1 is characterized in that: described halogen-free flame retardants is nitrogen system, nitrogen phosphorus system or phosphorus flame retardant, and above-mentioned substance is by the mixture of making a gesture of measuring combination arbitrarily.
8. the preparation method of a halogen-free flame-retardant nylon 6 material is characterized in that: concrete preparation process is as follows:
(1) major ingredient of preparation halogen-free flame-retardant nylon 6 material:
Nylon 6 pellets are put into high mixer, then thermo-stabilizer, oxidation inhibitor are put into high mixer, mix and stirred 2-5 minute, again mineral filler powder, modifier, pigment are put into high mixer and continued to mix stirring 2-5 minute, add halogen-free flame retardants mixing discharging after 2-5 minute at last, the material of emitting is the major ingredient of halogen-free flame-retardant nylon 6 material;
(2) preparation halogen-free flame-retardant nylon 6 material:
Major ingredient extruding pelletization on twin screw extruder with halogen-free flame-retardant nylon 6 material, one district's temperature is 220～250 ℃ from the spout to the die head, 225～250 ℃ of two district's temperature, 230～240 ℃ of three district's temperature, 235～250 ℃ of four district's temperature, 235～250 ℃ of five district's temperature, 220～240 ℃ of six district's temperature, 235～255 ℃ of seven district's temperature, 235～255 ℃ of eight district's temperature, 250 ℃ of head temperatures; Residence time is 0.5～2min, and engine speed is 200～440r/min, and pressure is 10～15MPa, through discharging, extrude postcooling, drying, pelletizing, the halogen-free flame-retardant nylon 6 material finished product.
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| CNA2009100315848A CN101565543A (en) | 2009-04-24 | 2009-04-24 | Halogen-free flame-retardant nylon 6 material and preparation method thereof |
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| CNA2009100315848A CN101565543A (en) | 2009-04-24 | 2009-04-24 | Halogen-free flame-retardant nylon 6 material and preparation method thereof |
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Cited By (13)
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|---|---|---|---|---|
| CN101845220A (en) * | 2010-05-06 | 2010-09-29 | 浙江新力塑料股份有限公司 | Inflaming retarding reinforced plastic and preparation method thereof |
| CN101914288A (en) * | 2010-08-30 | 2010-12-15 | 南京聚隆科技股份有限公司 | Nylon 6 mineral fiber composite material for automobile engine cover lid and preparation method thereof |
| CN101921472A (en) * | 2010-08-18 | 2010-12-22 | 苏州奔腾塑业有限公司 | High impact-resistant halogen-free flame-retardant reinforced nylon material and preparation method thereof |
| CN102040833A (en) * | 2010-12-01 | 2011-05-04 | 福建奥峰科技有限公司 | Halogen-free enhanced flame-retardant high-CTI value PA6 material for circuit breaker and preparation method thereof |
| CN103242651A (en) * | 2013-05-21 | 2013-08-14 | 苏州旭光聚合物有限公司 | Reinforced and modified PA (Polyamide)6 composite material |
| CN104098764A (en) * | 2013-04-09 | 2014-10-15 | 合肥杰事杰新材料股份有限公司 | Cast nylon 6 heatproof composite material and preparation method thereof |
| CN104559160A (en) * | 2013-10-09 | 2015-04-29 | 上海杰事杰新材料(集团)股份有限公司 | Wollastonite/nylon 610T composite material and preparation method thereof |
| CN105153685A (en) * | 2015-08-03 | 2015-12-16 | 苏州云舒新材料科技有限公司 | Insulated nylon material and preparation method thereof |
| CN106548825A (en) * | 2016-12-08 | 2017-03-29 | 应剑军 | A kind of glass fibre high temperature-resistant cable and preparation method thereof |
| CN106675004A (en) * | 2016-12-26 | 2017-05-17 | 安徽元通采暖科技有限公司 | Anti-scalding jacket for fireplace smoke discharge pipe |
| CN106782812A (en) * | 2016-12-08 | 2017-05-31 | 应剑军 | A kind of glass fiber flame retardant cable and preparation method thereof |
| CN108892947A (en) * | 2018-05-24 | 2018-11-27 | 暨南大学 | A kind of halogen-free flame-retarded heat-conducting nylon material |
| CN109535706A (en) * | 2018-10-18 | 2019-03-29 | 金旸（厦门）新材料科技有限公司 | A kind of Weather resistant halogen-free flame retardant enhancing nylon material and preparation method |
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2009
- 2009-04-24 CN CNA2009100315848A patent/CN101565543A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101845220A (en) * | 2010-05-06 | 2010-09-29 | 浙江新力塑料股份有限公司 | Inflaming retarding reinforced plastic and preparation method thereof |
| CN101921472A (en) * | 2010-08-18 | 2010-12-22 | 苏州奔腾塑业有限公司 | High impact-resistant halogen-free flame-retardant reinforced nylon material and preparation method thereof |
| CN101914288A (en) * | 2010-08-30 | 2010-12-15 | 南京聚隆科技股份有限公司 | Nylon 6 mineral fiber composite material for automobile engine cover lid and preparation method thereof |
| CN101914288B (en) * | 2010-08-30 | 2013-01-02 | 南京聚隆科技股份有限公司 | Nylon 6 mineral fiber composite material for automobile engine cover lid and preparation method thereof |
| CN102040833A (en) * | 2010-12-01 | 2011-05-04 | 福建奥峰科技有限公司 | Halogen-free enhanced flame-retardant high-CTI value PA6 material for circuit breaker and preparation method thereof |
| CN102040833B (en) * | 2010-12-01 | 2012-10-03 | 福建奥峰科技有限公司 | Halogen-free enhanced flame-retardant high-CTI value PA6 material for circuit breaker and preparation method thereof |
| CN104098764A (en) * | 2013-04-09 | 2014-10-15 | 合肥杰事杰新材料股份有限公司 | Cast nylon 6 heatproof composite material and preparation method thereof |
| CN103242651A (en) * | 2013-05-21 | 2013-08-14 | 苏州旭光聚合物有限公司 | Reinforced and modified PA (Polyamide)6 composite material |
| CN104559160A (en) * | 2013-10-09 | 2015-04-29 | 上海杰事杰新材料(集团)股份有限公司 | Wollastonite/nylon 610T composite material and preparation method thereof |
| CN105153685A (en) * | 2015-08-03 | 2015-12-16 | 苏州云舒新材料科技有限公司 | Insulated nylon material and preparation method thereof |
| CN106548825A (en) * | 2016-12-08 | 2017-03-29 | 应剑军 | A kind of glass fibre high temperature-resistant cable and preparation method thereof |
| CN106782812A (en) * | 2016-12-08 | 2017-05-31 | 应剑军 | A kind of glass fiber flame retardant cable and preparation method thereof |
| CN106675004A (en) * | 2016-12-26 | 2017-05-17 | 安徽元通采暖科技有限公司 | Anti-scalding jacket for fireplace smoke discharge pipe |
| CN108892947A (en) * | 2018-05-24 | 2018-11-27 | 暨南大学 | A kind of halogen-free flame-retarded heat-conducting nylon material |
| CN108892947B (en) * | 2018-05-24 | 2020-09-25 | 广州润锋科技股份有限公司 | Halogen-free flame-retardant heat-conducting nylon material |
| CN109535706A (en) * | 2018-10-18 | 2019-03-29 | 金旸（厦门）新材料科技有限公司 | A kind of Weather resistant halogen-free flame retardant enhancing nylon material and preparation method |
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Open date: 20091028 |