CN102558850A - Flame-retardant functional masterbatch special for nylon 6 and preparation method for masterbatch - Google Patents
Flame-retardant functional masterbatch special for nylon 6 and preparation method for masterbatch Download PDFInfo
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- CN102558850A CN102558850A CN2011104130778A CN201110413077A CN102558850A CN 102558850 A CN102558850 A CN 102558850A CN 2011104130778 A CN2011104130778 A CN 2011104130778A CN 201110413077 A CN201110413077 A CN 201110413077A CN 102558850 A CN102558850 A CN 102558850A
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Abstract
The invention relates to a flame-retardant functional masterbatch special for nylon 6 and a preparation method for the masterbatch. The conventional nylon 6 flame retardant influences the performance of the nylon 6 and is difficult to accurately add. The masterbatch is a mixture, and each 100 weight parts of masterbatch comprises the following raw materials in part by weight: 40 to 75 parts of main flame retardant, 3 to 20 parts of flame-retardant synergist, 20 to 40 parts of carrier resin, 0.4 to 2 parts of antioxidant, 0.5 to 3 parts of coupling agent and 0.5 to 5 parts of dispersing agent. The preparation method comprises the following steps of: adding the raw material components into a kneader in a ratio, stirring, uniformly mixing, taking out, and drying at the temperature of between 60 and 100 DEG C in vacuum to obtain a crude material; and melting, extruding and pelletizing the crude material by using a double-screw extruder to obtain a finished masterbatch product. The masterbatch can be directly added into a nylon 6 substrate in a ratio, effectively improves the flame retardance of a nylon 6 material, and cannot generate harmful gas during combustion; and the preparation method is easy to operate, low in energy consumption and suitable for industrial production.
Description
Technical field
The invention belongs to technical field of polymer materials, relate to a kind of nylon 6 special-purpose anti-flaming functional master batchs and preparation method thereof.
Technical background
Nylon 6 be used widely at aspects such as automobile, electricinstallation, Machinery Ministry structure, transportation equipment, weaving, papermaking equipments, but the shortcoming of flame retardant resistance extreme difference makes its application receive very big restriction because of its excellent mechanical property and drug-resistant corrodibility.
At present, generally be directly to add fire retardant to give nylon 6 flame retardant propertiess.Halogenated flame retardant is the high fire retardant of a kind of flame retarding efficiency, but its when burning can emit harmful gas, its application is restricted.Though the expanded polystyrene veneer of up-to-date exploitation and inorganic combustion inhibitor are environment friendly flame retardants; But reach good flame-retardant effect; Addition that must be big, the obvious deterioration of outward appearance, processing characteristics and physical and mechanical properties that this causes nylon 6 material or its goods influences the application of nylon 6 material.On the other hand, fire retardant and auxiliary agent all are powdery basically, in the course of processing of macromolecular material; Add fire retardant and other auxiliary agent item by item, brought inconvenience for actual processing and operations, for example; Be difficult for accurately control adding proportion, operator's labour protection hidden danger etc.
Therefore; Be necessary to develop a kind of nylon 6 special-purpose halogen-free flameproof functional master batchs; Can increase the flame retardant properties of nylon 6 material on the one hand; Adding multiple performance such as mechanical property, the thermostability etc. that these nylon 6 flame-retardant master batchs can not damage or hang down the infringement nylon 6 material on the other hand, also be convenient to simultaneously transport and process and use.
Summary of the invention
The purpose of this invention is to provide a kind of cheap, addition is low and add in the nylon-6 matrix body; Both can improve matrix flame retardant resistance and thermotolerance; Simultaneously nylon-6 matrix body favorable mechanical performance can be kept again, and the nylon 6 special-purpose halogen-free flameproof functional master batchs of matrix heat-drawn wire and barrier properties for gases can be obviously improved; Another object of the present invention provide a kind of simple to operate, energy consumption is low, is easy to the preparation method of suitability for industrialized production.
Nylon 6 special-purpose anti-flaming functional master batchs of the present invention are the mixture that main flame retardant, fire retarding synergist, vector resin, oxidation inhibitor, coupling agent and dispersion agent blend form;
Contain 40～75 parts of main flame retardants, 3～20 parts of fire retarding synergists, 20～40 parts of vector resins, 0.4～2 part in oxidation inhibitor, 0.5～3 part of coupling agent, 0.5～5 part of dispersion agent in the nylon 6 special-purpose anti-flaming functional master batchs of per 100 weight parts;
Described main flame retardant is at least a in Marinco H, red phosphorus, trimeric cyanamide, ammonium polyphosphate, the polyphosphoric acid melamine;
Described fire retarding synergist is at least a in zinc borate, zinc oxide, silicon-dioxide, ZGK 5, the fire-retardantization modified clay; Wherein, fire-retardantization modified clay is ripe commodity, and directly market is bought, for example fire-retardantization modified clay series FR-1, FR-2, the FR-3 of the production of Zhejiang Feng Hong novel material limited-liability company.
Described vector resin is a nylon 6;
Described oxidation inhibitor is four [β-(3; 5-di-t-butyl-4-hydroxyl) phenylpropionic acid] pentaerythritol ester (antioxidant 1010), β-(3; The 5-di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester (antioxidant 1076), three (2; The 4-di-tert-butyl-phenyl) at least a in phosphorous acid ester (oxidation inhibitor 168), two (2, the 4-DI-tert-butylphenol compounds) pentaerythritol diphosphites (oxidation inhibitor 626), two (octadecyl) pentaerythritol diphosphites (oxidation inhibitor 618);
Described coupling agent is at least a in γ-An Bingjisanyiyangjiguiwan (KH-550), γ-methacryloxypropyl trimethoxy silane (KH-570), sec.-propyl three (dioctyl phosphoryl) titanic acid ester (NSZ-20);
Described dispersion agent is at least a in calcium stearate, Zinic stearas, the polyethylene wax;
The concrete grammar for preparing these nylon 6 special-purpose anti-flaming functional master batchs is: add main flame retardant, fire retarding synergist, oxidation inhibitor, coupling agent, dispersion agent and vector resin in the kneader in proportion; Mix; Play the material back in 60～100 ℃ of oven dry down of vacuum, become coarse fodder; With coarse fodder through the twin screw extruder fusion, extrude, granulation, make the masterbatch finished product.
The present invention is through to main flame retardant, fire retarding synergist and vector resin preferably, with the twin screw extruder melt pelletization, make a kind of nylon 6 special-purpose anti-flaming functional master batchs.Flame-retardant master batch through the present invention's preparation can directly add in the nylon-6 matrix body in proportion, improves the flame retardant properties of nylon 6 material.Simultaneously, these nylon 6 special-purpose anti-flaming functional master batchs are not halogen-containing, can not emit obnoxious flavour during burning.
Compare with present common fire retardant material; Anti-flaming function nylon 6 masterbatch of the present invention have the body material of raising flame retardant properties simultaneously and keep matrix favorable mechanical performance, and can obviously improve matrix heat-drawn wire and barrier properties for gases and the convenient characteristics of using.
Embodiment
Embodiment 1
400g polyphosphoric acid melamine, fire-retardantization of 200gFR-1 Feng Hong modified clay, 380g nylon 6,4g antioxidant 1076,7g coupling agent KH-550,9g calcium stearate are added in the kneader; Mix; Play the material back in 60 ℃ of oven dry down of vacuum; Then through the twin screw extruder fusion, extrude, granulation, make 1000g nylon 6 special-purpose anti-flaming functional master batch finished products.
Embodiment 2
450g red phosphorus, 100g zinc borate, 400g nylon 6,20g antioxidant 1010,5g coupling agent kh-570,25g Zinic stearas are added in the kneader; Mix; Play the material back in 80 ℃ of oven dry down of vacuum; Then through the twin screw extruder fusion, extrude, granulation, make 1000g nylon 6 special-purpose anti-flaming functional master batch finished products.
Embodiment 3
550g trimeric cyanamide, 150g zinc oxide, 250g nylon 6,4g antioxidant 1076,1g oxidation inhibitor 626,17g coupling agent NSZ-20,28g polyethylene wax are added in the kneader; Mix; Play the material back in 90 ℃ of oven dry down of vacuum; Then through the twin screw extruder fusion, extrude, granulation, make 1000g nylon 6 special-purpose anti-flaming functional master batch finished products.
Embodiment 4
720g ammonium polyphosphate, 30g silicon-dioxide, 225g nylon 6,6g antioxidant 1010,2g oxidation inhibitor 168,12g coupling agent kh-570,5g calcium stearate are added in the kneader; Mix; Play the material back in 100 ℃ of oven dry down of vacuum; Then through the twin screw extruder fusion, extrude, granulation, make 1000g nylon 6 special-purpose anti-flaming functional master batch finished products.
Embodiment 5
750g Marinco H, 30g ZGK 5,200g nylon 6,5g antioxidant 1010,5g coupling agent KH-550,5g Zinic stearas, 5g calcium stearate are added in the kneader; Mix; Play the material back in 85 ℃ of oven dry down of vacuum; Then through the twin screw extruder fusion, extrude, granulation, make 1000g nylon 6 special-purpose anti-flaming functional master batch finished products.
Embodiment 6
200g trimeric cyanamide, 200g ammonium polyphosphate, 115g zinc borate, 400g nylon 6,5g antioxidant 1076,30g coupling agent KH-550,50g polyethylene wax are added in the kneader; Mix; Play the material back in 75 ℃ of oven dry down of vacuum; Then through the twin screw extruder fusion, extrude, granulation, make 1000g nylon 6 special-purpose anti-flaming functional master batch finished products.
Embodiment 7
550g red phosphorus, 100g zinc borate, 100g zinc oxide, 200g nylon 6,4g antioxidant 1076,16g coupling agent NSZ-20,30g polyethylene wax are added in the kneader; Mix; Play the material back in 65 ℃ of oven dry down of vacuum; Then through the twin screw extruder fusion, extrude, granulation, make 1000g nylon 6 special-purpose anti-flaming functional master batch finished products.
Embodiment 8
500g polyphosphoric acid melamine, fire-retardantization of 200gFR-2 Feng Hong modified clay, 265g nylon 6,7g antioxidant 1010,9g coupling agent KH-550,9g coupling agent kh-570,10g Zinic stearas are added in the kneader; Mix; Play the material back in 95 ℃ of oven dry down of vacuum; Then through the twin screw extruder fusion, extrude, granulation, make 1000g nylon 6 special-purpose anti-flaming functional master batch finished products.
Embodiment 9
550g polyphosphoric acid melamine, fire-retardantization of 145gFR-3 Feng Hong modified clay, 270g nylon 6,7g antioxidant 1010,9g coupling agent KH-550,9g coupling agent kh-570,10g calcium stearate are added in the kneader; Mix; Play the material back in 80 ℃ of oven dry down of vacuum; Then through the twin screw extruder fusion, extrude, granulation, make 1000g nylon 6 special-purpose anti-flaming functional master batch finished products.
Embodiment 10
450g polyphosphoric acid melamine, fire-retardantization of 100gFR-1 Feng Hong modified clay, 100g series 2 fire-retardantization of Feng Hong modified clays, 300g nylon 6,3g antioxidant 1076,2g oxidation inhibitor 618,25g coupling agent NSZ-20,20g Zinic stearas are added in the kneader; Mix; Play the material back in 75 ℃ of oven dry down of vacuum; Then through the twin screw extruder fusion, extrude, granulation, make 1000g nylon 6 special-purpose anti-flaming functional master batch finished products.
Table 1. flame-retardant master batch flame-proof PA 6 performance comparison sheet
Data through table 1 can find out that after the nylon 6 special-purpose anti-flaming functional master batchs of preparation added the nylon-6 matrix body to, its flame retardant properties all can reach V-0, and will be much better than commercial flame retardant PA6 matrix in mechanical property.
Claims (2)
1. nylon 6 special-purpose anti-flaming functional master batchs, the mixture for main flame retardant, fire retarding synergist, vector resin, oxidation inhibitor, coupling agent and dispersion agent blend form is characterized in that:
Contain 40～75 parts of main flame retardants, 3～20 parts of fire retarding synergists, 20～40 parts of vector resins, 0.4～2 part in oxidation inhibitor, 0.5～3 part of coupling agent, 0.5～5 part of dispersion agent in the nylon 6 special-purpose anti-flaming functional master batchs of per 100 weight parts;
Described main flame retardant is at least a in Marinco H, red phosphorus, trimeric cyanamide, ammonium polyphosphate, the polyphosphoric acid melamine;
Described fire retarding synergist is at least a in zinc borate, zinc oxide, silicon-dioxide, ZGK 5, the fire-retardantization modified clay;
Described vector resin is a nylon 6;
Described oxidation inhibitor is four [β-(3; 5-di-t-butyl-4-hydroxyl) phenylpropionic acid] pentaerythritol ester, β-(3; The 5-di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester, three (2; The 4-di-tert-butyl-phenyl) at least a in phosphorous acid ester, two (2, the 4-DI-tert-butylphenol compounds) pentaerythritol diphosphites, two (octadecyl) pentaerythritol diphosphites;
Described coupling agent is at least a in γ-An Bingjisanyiyangjiguiwan, γ-methacryloxypropyl trimethoxy silane, sec.-propyl three (dioctyl phosphoryl) titanic acid ester;
Described dispersion agent is at least a in calcium stearate, Zinic stearas, the polyethylene wax.
2. the preparation method of nylon 6 special-purpose anti-flaming functional master batchs; It is characterized in that: add main flame retardant, fire retarding synergist, oxidation inhibitor, coupling agent, dispersion agent and vector resin in the kneader in proportion; Mix, play the material back, become coarse fodder in 60～100 ℃ of oven dry down of vacuum; With coarse fodder through the twin screw extruder fusion, extrude, granulation, make the masterbatch finished product;
Described main flame retardant is at least a in Marinco H, red phosphorus, trimeric cyanamide, ammonium polyphosphate, the polyphosphoric acid melamine;
Described fire retarding synergist is at least a in zinc borate, zinc oxide, silicon-dioxide, ZGK 5, the fire-retardantization modified clay;
Described vector resin is a nylon 6;
Described oxidation inhibitor is four [β-(3; 5-di-t-butyl-4-hydroxyl) phenylpropionic acid] pentaerythritol ester, β-(3; The 5-di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester, three (2; The 4-di-tert-butyl-phenyl) at least a in phosphorous acid ester, two (2, the 4-DI-tert-butylphenol compounds) pentaerythritol diphosphites, two (octadecyl) pentaerythritol diphosphites;
Described coupling agent is at least a in γ-An Bingjisanyiyangjiguiwan, γ-methacryloxypropyl trimethoxy silane, sec.-propyl three (dioctyl phosphoryl) titanic acid ester;
Described dispersion agent is at least a in calcium stearate, Zinic stearas, the polyethylene wax;
The nylon 6 special-purpose anti-flaming functional master batchs that prepare 100 weight parts add 40～75 parts of main flame retardants, 3～20 parts of fire retarding synergists, 20～40 parts of vector resins, 0.4～2 part in oxidation inhibitor, 0.5～3 part of coupling agent, 0.5～5 part of dispersion agent.
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| CN102877988A (en) * | 2012-09-27 | 2013-01-16 | 蚌埠市昊业滤清器有限公司 | Threaded cover plate |
| CN103435952A (en) * | 2013-07-30 | 2013-12-11 | 浙江万盛股份有限公司 | Phosphate nano composite flame-retardant masterbatch and preparation method thereof |
| CN103642214A (en) * | 2013-11-18 | 2014-03-19 | 安徽宜万丰电器有限公司 | Low-cost flame-retardant modified nylon material for automobile plastic members |
| CN104592751A (en) * | 2014-12-10 | 2015-05-06 | 苏州博利迈新材料科技有限公司 | Halogen-free flame retardant reinforced nylon 612 composite material, preparation method and application thereof |
| CN105038242A (en) * | 2015-07-06 | 2015-11-11 | 刘雷 | Organosilicon fire retardant and preparation method thereof |
| CN105038238A (en) * | 2015-07-03 | 2015-11-11 | 安徽扬子化工有限公司 | Preparation method of organic silicon fire retardant of organic silicon rubber wastes |
| CN105542305A (en) * | 2016-01-25 | 2016-05-04 | 上海捷棉新材料科技有限公司 | Halogen-free high-temperature-resisting flame-resistant material high in oxygen index and preparation method and application thereof |
| CN106987029A (en) * | 2017-05-10 | 2017-07-28 | 浙江鹏远新材料股份有限公司 | Flame retardant of magnesium hydroxide and preparation method thereof and flame-retardant crosslinking polyethylene foamed plastics |
| CN107353647A (en) * | 2016-05-10 | 2017-11-17 | 合肥杰事杰新材料股份有限公司 | A kind of low smell, low distribute carrier-free nano flame-proof agglomerate and preparation method thereof |
| CN107686595A (en) * | 2017-11-09 | 2018-02-13 | 陕西汉中卓尔新材料科技有限公司 | A kind of red phosphorus flame-retardant masterbatch and its manufacture method |
| CN110511430A (en) * | 2019-08-19 | 2019-11-29 | 广东顺亨新材料有限公司 | A kind of fire retarding synergist and preparation method thereof of alternative antimony oxide |
| US11401416B2 (en) | 2017-10-17 | 2022-08-02 | Celanese Sales Germany Gmbh | Flame retardant polyamide composition |
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| CN102877988A (en) * | 2012-09-27 | 2013-01-16 | 蚌埠市昊业滤清器有限公司 | Threaded cover plate |
| CN103435952A (en) * | 2013-07-30 | 2013-12-11 | 浙江万盛股份有限公司 | Phosphate nano composite flame-retardant masterbatch and preparation method thereof |
| CN103435952B (en) * | 2013-07-30 | 2015-08-05 | 浙江万盛股份有限公司 | A kind of Phosphate nano composite flame-retardant masterbatch and preparation method thereof |
| CN103642214A (en) * | 2013-11-18 | 2014-03-19 | 安徽宜万丰电器有限公司 | Low-cost flame-retardant modified nylon material for automobile plastic members |
| CN104592751A (en) * | 2014-12-10 | 2015-05-06 | 苏州博利迈新材料科技有限公司 | Halogen-free flame retardant reinforced nylon 612 composite material, preparation method and application thereof |
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| CN105038242A (en) * | 2015-07-06 | 2015-11-11 | 刘雷 | Organosilicon fire retardant and preparation method thereof |
| CN105038242B (en) * | 2015-07-06 | 2017-03-29 | 湖北工业大学 | Organic silicon fibre retardant and preparation method thereof |
| CN105542305A (en) * | 2016-01-25 | 2016-05-04 | 上海捷棉新材料科技有限公司 | Halogen-free high-temperature-resisting flame-resistant material high in oxygen index and preparation method and application thereof |
| CN107353647A (en) * | 2016-05-10 | 2017-11-17 | 合肥杰事杰新材料股份有限公司 | A kind of low smell, low distribute carrier-free nano flame-proof agglomerate and preparation method thereof |
| CN106987029A (en) * | 2017-05-10 | 2017-07-28 | 浙江鹏远新材料股份有限公司 | Flame retardant of magnesium hydroxide and preparation method thereof and flame-retardant crosslinking polyethylene foamed plastics |
| US11401416B2 (en) | 2017-10-17 | 2022-08-02 | Celanese Sales Germany Gmbh | Flame retardant polyamide composition |
| CN107686595A (en) * | 2017-11-09 | 2018-02-13 | 陕西汉中卓尔新材料科技有限公司 | A kind of red phosphorus flame-retardant masterbatch and its manufacture method |
| CN110511430A (en) * | 2019-08-19 | 2019-11-29 | 广东顺亨新材料有限公司 | A kind of fire retarding synergist and preparation method thereof of alternative antimony oxide |
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Application publication date: 20120711 |