CN104448803B - Halogen-free flame-retardant long-fiber-reinforced nylon 6 composite material and preparation method thereof - Google Patents
Halogen-free flame-retardant long-fiber-reinforced nylon 6 composite material and preparation method thereof Download PDFInfo
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- CN104448803B CN104448803B CN201410708756.1A CN201410708756A CN104448803B CN 104448803 B CN104448803 B CN 104448803B CN 201410708756 A CN201410708756 A CN 201410708756A CN 104448803 B CN104448803 B CN 104448803B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Abstract
The invention discloses a halogen-free flame-retardant long-fiber-reinforced nylon 6 composite material. Nylon 6 is taken as matrix resin, SMA (styrene maleic anhydride) is taken as a compatilizer which reinforces the binding force between the matrix resin and fiber, and one-step method is adopted for preparation of the halogen-free flame-retardant long-fiber-reinforced nylon 6 composite material; and according to the preparation method, continuous fiber is impregnated by the matrix resin through an impregnation mold, an impregnation bar is coated with a matrix melt, containing a halogen-free flame retardant, in a coating mold, then cooling and traction are performed, and finally, the material is cut to required length by a granulator. The production technology is simple, a prepared product has excellent mechanical properties and is quite environment-friendly, and the problem of a floating fiber phenomenon when nylon is reinforced by glass fiber is solved.
Description
Technical field
The present invention relates to technical field of polymer materials, especially a kind of halogen-free flameproof long fiber reinforced Nylon 6 composite wood
Material and preparation method thereof.
Background technology
Nylon 6 is a kind of engineering plastics being widely used in the industries such as automobile, electronics, decoration.Due to its special chemistry
Structure, pure nylon 6 can produce substantial amounts of molten drop in combustion and take away heat and material, thus itself is in combustion process
In possess certain self-extinguishment.But this self-extinguishment acts in nylon 6 composite material not to be occurred, and in enhancement mode
In nylon 6 composite material, molten drop self-extinguishment mechanism can be acted on to fire-retardant forfeiture due to ' candle wick effect '.It is thus desirable to hindering to it
Combustion is modified；Today's society, the awareness of safety of people improves, and the environmental protection concept of country is constantly strengthened, and therefore, is hindered using Halogen
It is very important problem that fire proofing is prepared in combustion agent.Due to the requirement more and more higher to product quality for the people, common short fibre
The performance of dimension reinforced nylon 6 material can not meet requirement, and can produce " floating fibre " phenomenon, and long fiber reinforced Nylon 6 has high-strength
The excellent performance such as degree, high-modulus, high thermal stability can meet people and high-performance is pursued, and is preparing fire-retardant long fiber reinforcement
During thermoplastic composite, traditional method be two-step method (that is: prepare fire-retardant master granule and long fiber reinforcement master batch first respectively,
Then mix and be molded).
Content of the invention
The purpose of the present invention is: provides a kind of high-performance halogen-free flame retardant long fiber reinforced Nylon 6 composite and its preparation
Method, it solves the problems, such as that nylon 6 is readily burned, and effectively increases the mechanical property of product, and environment protecting is good, simultaneously
Solve " floating fibre " phenomenon of glass fiber reinforced nylon 6, and preparation method is simple, to overcome the deficiencies in the prior art.
The present invention is achieved in that halogen-free flameproof long fiber reinforced Nylon 6 composite, calculates according to the mass fraction, bag
Include 80-100 part nylon 6,40-50 part fiber, 8-12 part compatilizer, 0.8-1.2 part antioxidant, 25-35 part halogen-free flame retardants, 8-
12 portions of synergist, 17-22 part carbon forming agent and 1-3 part dispersant.
Described fiber is ramee, tossa, flax fiber, hemp, glass fibre, kenaf, sword
Any combination of one or more of flaxen fiber or bamboo fibre.
Described compatilizer is SMA.
Described halogen-free flame retardants is aluminum phenylphosphinate.
Described synergist is quaternary alkylphosphonium salt intercalated montmorillonite.
Described Si modification phenolic aldehyde carbon forming agent, described dispersant is pentaerythritol stearate.
The preparation method of halogen-free flameproof long fiber reinforced Nylon 6 composite, takes 45-55 part nylon 6 and 4-6 part phase respectively
Hold agent drying for standby, above-mentioned dried nylon 6 and compatilizer, 0.4-0.6 part antioxidant are mixed, is then blended
Extrusion, processing temperature is 150-200 DEG C, and melt is impregnated to 40-50 part fiber by impregnating runner, obtains fiber impregnation
Material strip；Take 35-45 part nylon 6,25-35 part halogen-free flame retardants, 8-12 portions of synergist, 17-22 part carbon forming agent, the dispersion of 1-3 part again
Agent and 4-6 part compatilizer are dried, and above-mentioned dried material is mixed with 0.4-0.6 part antioxidant, material is mixed
Close and uniformly add afterwards in extruder, in extrusion, the mixed material of melting is coated in fiber impregnation material strip, pelletizing after cooling
Become the particle of 8～12mm, obtain halogen-free flameproof long fiber reinforced Nylon 6 composite.
Described baking temperature is 60-80 DEG C, and drying time is 5-8h.
In the present invention, what dipping runner and be coated on the mixed material of melting was adopted in fiber impregnation material strip sets
Standby, it is the device disclosed in the application for a patent for invention of Application No. " 201110453139.8 " of applicant's earlier application, that is,
Realize the device of continuous roving glass fiber extrusion.
Due to employing technique scheme, compared with prior art, the present invention adopts nylon 6 as matrix resin, with
Sma enhances the adhesion between matrix resin and fiber as compatilizer, this compatilizer, and prepares Halogen resistance using one-step method
Combustion long fiber reinforced Nylon 6 composite, continuously will complete the dipping to fiber for the matrix resin by impregnation mold by fiber,
Then complete matrix melt with the halogen-free flame retardants cladding in dipping material strip in coating mould, then carry out cooling down,
Draw, be cut into Len req finally by pelleter, compared with existing two-step method, such mode not only process is simple, and
And prepared product mechanical property is excellent, environment-friendly type is good, and solves " floating fibre " phenomenon easily occurring during glass fiber enhanced nylon.This
Invention is simple, material source is extensive, with low cost, and using effect is good.
Brief description
Accompanying drawing 1 is the flow chart of the present invention.
Specific embodiment
Embodiments of the invention 1: halogen-free flameproof long fiber reinforced Nylon 6 composite, calculate according to the mass fraction, including 90
Part 6,45 parts of fibers of nylon, 10 parts of compatilizers, 1 part of antioxidant, 30 parts of halogen-free flame retardants, 10 portions of synergist, 20 parts of carbon forming agents with
And 2 parts of dispersants；Described fiber is glass fibre；Described compatilizer is SMA；Described
Halogen-free flame retardants be aluminum phenylphosphinate；Described synergist is quaternary alkylphosphonium salt intercalated montmorillonite；Described Si modification phenolic aldehyde becomes
Charcoal agent, described dispersant is pentaerythritol stearate.
The preparation method of halogen-free flameproof long fiber reinforced Nylon 6 composite, takes 40 parts of nylon 6 and 5 parts of compatilizers respectively
Drying for standby, above-mentioned dried nylon 6 and compatilizer, 0.5 part of antioxidant is mixed, then carries out blending extrusion, plus
Work temperature is 180 DEG C, and melt is impregnated to 45 parts of fibers by impregnating runner, obtains fiber impregnation material strip；Take 40 parts again
6,30 parts of halogen-free flame retardants of nylon, 10 portions of synergist, 20 parts of carbon forming agents, 2 parts of dispersants and 5 parts of compatilizers are dried, will be upper
State dried material to be mixed with 0.5 part of antioxidant, add after material is mixed in extruder, will melt in extrusion
The mixed material melting is coated in fiber impregnation material strip, and pelletizing after cooling becomes the particle of 8～12mm, obtains halogen-free flameproof long fibre
Reinforced nylon 6 composite；Described baking temperature is 70 DEG C, and drying time is 6h.
Embodiments of the invention 2: halogen-free flameproof long fiber reinforced Nylon 6 composite, calculate according to the mass fraction, including 80
Part 6,50 parts of fibers of nylon, 12 parts of compatilizers, 0.8 part of antioxidant, 25 parts of halogen-free flame retardants, 12 portions of synergist, 22 parts of carbon forming agents
And 1 part of dispersant；Described fiber is ramee；Described compatilizer is SMA；Institute
The halogen-free flame retardants stated is aluminum phenylphosphinate；Described synergist is quaternary alkylphosphonium salt intercalated montmorillonite；Described Si modification phenolic aldehyde
Carbon forming agent, described dispersant is pentaerythritol stearate.
The preparation method of halogen-free flameproof long fiber reinforced Nylon 6 composite, takes 45 parts of nylon 6 and 6 parts of compatilizers respectively
Drying for standby, above-mentioned dried nylon 6 and compatilizer, 0.4 part of antioxidant is mixed, then carries out blending extrusion, plus
Work temperature is 150 DEG C, and melt is impregnated to 50 parts of fibers by impregnating runner, obtains fiber impregnation material strip；Take 35 parts again
6,25 parts of halogen-free flame retardants of nylon, 12 portions of synergist, 22 parts of carbon forming agents, 1 part of dispersant and 6 parts of compatilizers are dried, will be upper
State dried material to be mixed with 0.4 part of antioxidant, add after material is mixed in extruder, will melt in extrusion
The mixed material melting is coated in fiber impregnation material strip, and pelletizing after cooling becomes the particle of 8～12mm, obtains halogen-free flameproof long fibre
Reinforced nylon 6 composite；Described baking temperature is 60 DEG C, and drying time is 8h.
Embodiments of the invention 3: halogen-free flameproof long fiber reinforced Nylon 6 composite, calculate according to the mass fraction, including
6,40 parts of fibers of 100 parts of nylon, 8 parts of compatilizers, 1.2 parts of antioxidant, 35 parts of halogen-free flame retardants, 8 portions of synergist, 17 parts of carbon forming agents
And 3 parts of dispersants；Described fiber is bamboo fibre；Described compatilizer is SMA；Described
Halogen-free flame retardants be aluminum phenylphosphinate；Described synergist is quaternary alkylphosphonium salt intercalated montmorillonite；Described Si modification phenolic aldehyde becomes
Charcoal agent, described dispersant is pentaerythritol stearate.
The preparation method of halogen-free flameproof long fiber reinforced Nylon 6 composite, takes 55 parts of nylon 6 and 4 parts of compatilizers respectively
Drying for standby, above-mentioned dried nylon 6 and compatilizer, 0.6 part of antioxidant is mixed, then carries out blending extrusion, plus
Work temperature is 200 DEG C, and melt is impregnated to 40 parts of fibers by impregnating runner, obtains fiber impregnation material strip；Take 45 parts again
6,35 parts of halogen-free flame retardants of nylon, 8 portions of synergist, 17 parts of carbon forming agents, 3 parts of dispersants and 4 parts of compatilizers are dried, will be above-mentioned
Dried material is mixed with 0.6 part of antioxidant, adds in extruder after material is mixed, and will melt in extrusion
Mixed material be coated in fiber impregnation material strip, pelletizing after cooling becomes the particle of 8～12mm, obtains halogen-free flameproof long fibre and increases
Strong nylon 6 composite material；Described baking temperature is 80 DEG C, and drying time is 5h.
In above-described embodiment, the trade mark of nylon 6 is 4042d；The trade mark of toughener is wb271；The trade mark of glass fibre is
er4301h；The trade mark of compatilizer is 1013b；The trade mark of antioxidant is as4500；Antioxidant is 168 or 1098.
Main performance is tested: the product produced makes standard testing batten according to standard, carries out every test, its performance
Test result is as shown in table 1.
Table 1
| Test event | Embodiment one | Embodiment two | Embodiment three |
| Tensile strength (mpa) | 180 | 195 | 171 |
| Izod notched impact strength (kj/m2) | 26.6 | 29.3 | 24.1 |
| Bending strength (mpa) | 247 | 260 | 238 |
| Fire resistance (ul94) | v0 | v0 | v0 |
| Shaping complexity | Easily | Easily | Easily |
| Surface quality | No decorative pattern | No decorative pattern | No decorative pattern |
According to table 1 it is known that adopting the preparation-obtained sample of technical scheme, with conventional nylon 6 material
Material is compared, and its performance is good, and intensity is high, solves " floating fibre " phenomenon of short fiber reinforced nylon 6 composite, and fire resistance is excellent
Different.
Claims (5)
1. a kind of halogen-free flameproof long fiber reinforced Nylon 6 composite it is characterised in that: calculate according to the mass fraction, including 80-
100 parts of nylon 6,40-50 part fiber, 8-12 part compatilizer, 0.8-1.2 part antioxidant, 25-35 part halogen-free flame retardants, 8-12 parts
Synergist, 17-22 part carbon forming agent and 1-3 part dispersant, its preparation method is: takes 45-55 part nylon 6 and 4-6 part phase respectively
Hold agent drying for standby, above-mentioned dried nylon 6 and compatilizer, 0.4-0.6 part antioxidant are mixed, is then blended
Extrusion, processing temperature is 150-200 DEG C, and melt is impregnated to 40-50 part fiber by impregnating runner, obtains fiber impregnation
Material strip；Take 35-45 part nylon 6,25-35 part halogen-free flame retardants, 8-12 portions of synergist, 17-22 part carbon forming agent, the dispersion of 1-3 part again
Agent and 4-6 part compatilizer are dried, and above-mentioned dried material is mixed with 0.4-0.6 part antioxidant, material is mixed
Close and uniformly add afterwards in extruder, in extrusion, the mixed material of melting is coated in fiber impregnation material strip, pelletizing after cooling
Become the particle of 8～12mm, obtain halogen-free flameproof long fiber reinforced Nylon 6 composite；Described halogen-free flame retardants is phenyl
Phosphonic acids aluminium；Described synergist is quaternary alkylphosphonium salt intercalated montmorillonite；Described carbon forming agent is Si modification phenolic aldehyde carbon forming agent, and described divides
Powder is pentaerythritol stearate.
2. halogen-free flameproof long fiber reinforced Nylon 6 composite according to claim 1 it is characterised in that: described fibre
Tie up as in ramee, tossa, flax fiber, hemp, glass fibre, kenaf, sisal fiber or bamboo fibre
Any combination of one or more.
3. halogen-free flameproof long fiber reinforced Nylon 6 composite according to claim 1 it is characterised in that: described phase
Appearance agent is SMA.
4. a kind of preparation method of halogen-free flameproof long fiber reinforced Nylon 6 composite as claimed in claim 1, its feature exists
In: take 45-55 part nylon 6 and 4-6 part compatilizer drying for standby respectively, by above-mentioned dried nylon 6 and compatilizer, 0.4-
0.6 part of antioxidant mixes, and then carries out blending extrusion, and processing temperature is 150-200 DEG C, and melt is passed through to impregnate runner pair
40-50 part fiber is impregnated, and obtains fiber impregnation material strip；Take 35-45 part nylon 6,25-35 part halogen-free flame retardants, 8-12 again
Portions of synergist, 17-22 part carbon forming agent, 1-3 part dispersant and 4-6 part compatilizer are dried, by above-mentioned dried material with
0.4-0.6 part antioxidant is mixed, and adds in extruder after material is mixed, in extrusion by the mixed material of melting
It is coated in fiber impregnation material strip, pelletizing after cooling becomes the particle of 8～12mm, obtains halogen-free flameproof long fiber reinforced Nylon 6 multiple
Condensation material.
5. the preparation method of halogen-free flameproof long fiber reinforced Nylon 6 composite according to claim 4, its feature exists
In: baking temperature is 60-80 DEG C, and drying time is 5-8h.
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| CN201410708756.1A CN104448803B (en) | 2014-12-01 | 2014-12-01 | Halogen-free flame-retardant long-fiber-reinforced nylon 6 composite material and preparation method thereof |
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| CN106398204A (en) * | 2016-09-04 | 2017-02-15 | 康命源（安徽）塑料科技发展股份有限公司 | Halogen-free flame-retardant long-glass-fiber reinforced nylon 46 composite material and preparation method thereof |
| CN106380841A (en) * | 2016-09-04 | 2017-02-08 | 康命源（安徽）塑料科技发展股份有限公司 | Halogen-free and flame-retardant long glass fiber reinforced nylon 66 composite material and preparation method thereof |
| CN106317865A (en) * | 2016-09-04 | 2017-01-11 | 康命源（安徽）塑料科技发展股份有限公司 | Halogen-free flame-retardant glass fiber reinforced nylon 6 composite material and preparation method thereof |
| CN106398191A (en) * | 2016-09-04 | 2017-02-15 | 康命源（安徽）塑料科技发展股份有限公司 | Halogen-free flame-retardant long glass fiber enhanced nylon 6T composite material and preparation method thereof |
| CN106479165A (en) * | 2016-09-30 | 2017-03-08 | 宋兰兰 | Halogen-free flame-retardant long fiberglass reinforced PA 6 composite and its one-step preppn process |
| CN106479172A (en) * | 2016-09-30 | 2017-03-08 | 田晴晴 | Halogen-free flameproof long glass fiber reinforced is high temperature resistant PA6T composite 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 |
| CN106675005A (en) * | 2016-12-27 | 2017-05-17 | 上海普利特复合材料股份有限公司 | Long hemp fiber reinforced nylon composite material and preparation method thereof |
| CN114045043B (en) * | 2021-11-30 | 2022-11-04 | 浙江远景体育用品股份有限公司 | High-impact wood-plastic helmet composite material and preparation method thereof |
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| EP1340790A3 (en) * | 1995-12-22 | 2003-10-22 | E.I. Du Pont De Nemours And Company | Flame retardant polyamide compositions |
| US5618865A (en) * | 1995-12-22 | 1997-04-08 | E. I. Du Pont De Nemours And Company | Fire resistant resin compositions |
| JP5243006B2 (en) * | 2006-12-04 | 2013-07-24 | 三菱エンジニアリングプラスチックス株式会社 | Flame retardant polyamide resin composition and molded article |
| CN101792602A (en) * | 2010-03-11 | 2010-08-04 | 四川大学 | Halogen-free expansible flame-retardant thermoplastic resin composition |
| CN102838098A (en) * | 2011-06-24 | 2012-12-26 | 中国科学技术大学苏州研究院 | Rare earth metal hypophosphite and preparation method and application of rare earth metal hypophosphite |
| CN102504529B (en) * | 2011-11-17 | 2014-03-05 | 常州大学 | Halogen-free flame-retardant long glass fiber reinforced nylon 6 material and preparation method thereof |
| CN102634181B (en) * | 2012-04-25 | 2013-09-04 | 中国科学院宁波材料技术与工程研究所 | Catalytic flame retardant polylactic acid composite material |
| CN103937229A (en) * | 2013-01-17 | 2014-07-23 | 上海杰事杰新材料(集团)股份有限公司 | Fire retardant glass fiber reinforced nylon composite material, and preparation method thereof |
| CN103737736B (en) * | 2014-01-09 | 2016-04-27 | 朱建一 | Preparation facilities of a kind of long fiber reinforcement thermoplastic composite resin granular material and preparation method thereof |
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Denomination of invention: Halogen free flame retardant long fiber reinforced nylon 6 composite and its preparation method Effective date of registration: 20201221 Granted publication date: 20170125 Pledgee: Baiyun branch of Guiyang Bank Co.,Ltd. Pledgor: GUIZHOU KUMKUAT MATERIALS Ltd. Registration number: Y2020980009634 |
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Date of cancellation: 20220518 Granted publication date: 20170125 Pledgee: Baiyun branch of Guiyang Bank Co.,Ltd. Pledgor: GUIZHOU KUMKUAT MATERIALS Ltd. Registration number: Y2020980009634 |