CN104448803A - 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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- CN104448803A CN104448803A CN201410708756.1A CN201410708756A CN104448803A CN 104448803 A CN104448803 A CN 104448803A CN 201410708756 A CN201410708756 A CN 201410708756A CN 104448803 A CN104448803 A CN 104448803A
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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
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 matrix 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 the chemical structure that it is special, pure nylon 6 can produce a large amount of molten drops in combustion and take away heat and material, and thus itself possesses certain self-extinguishment in combustion.But thisly not occur from putting out to act in nylon 6 matrix material, and molten drop can act on fire-retardant forfeiture due to ' candle wick effect ' from putting out mechanism in nylon 6 matrix material of enhancement type.Therefore need to carry out flame-retardant modified to it; Society, the awareness of safety of people improves, and the environmental protection concept of country is constantly strengthened, and therefore, using halogen-free flame retardants to prepare fire retardant material is very important problem.Because the requirement of people to quality product is more and more higher, the performance of common short fiber reinforced nylon 6 material can not meet the demands, and " floating fine " phenomenon can be produced, long fiber reinforced Nylon 6 has the excellent performance such as high strength, high-modulus, high thermal stability and can meet people to high-performance and pursue, when preparing fire-retardant long fiber reinforced thermoplastic composites, traditional method is two-step approach (that is: prepares fire-retardant master granule and long fiber reinforcement master batch first respectively, then mix and carry out injection moulding).
Summary of the invention
The object of the invention is: a kind of high-performance halogen-free flame retardant long fiber reinforcement lactic acid composite material and preparation method thereof is provided, it solve the problem that nylon 6 is easy to burn, and effectively improve the mechanical property of product, environment protecting is good, solve " floating fine " phenomenon of glass fiber reinforced nylon 6 simultaneously, 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 matrix material, calculate according to the mass fraction, comprise 80-100 part nylon 6,40-50 part fiber, 8-12 part compatilizer, 0.8-1.2 part oxidation inhibitor, 25-35 part halogen-free flame retardants, 8-12 portions of synergist, 17-22 part char-forming agent and 1-3 part dispersion agent.
Described fiber is the arbitrary combination of one or more in ramee, jute fibre, flax fiber, hemp fibre, glass fibre, kenaf, sisal fibers or bamboo fibers.
Described compatilizer is styrene maleic anhydride copolymer.
Described halogen-free flame retardants is aluminum phenylphosphinate.
Described synergist is quaternary alkylphosphonium salt intercalated montmorillonite.
Described Si modification phenolic aldehyde char-forming agent, described dispersion agent is tetramethylolmethane stearate.
The preparation method of halogen-free flameproof long fiber reinforced Nylon 6 matrix material, get 45-55 part poly(lactic acid) and 4-6 part compatilizer drying for standby respectively, above-mentioned dried poly(lactic acid) and compatilizer 0.4-0.6 part oxidation inhibitor are mixed, then blending extrusion is carried out, processing temperature is 150-200 DEG C, melt is flooded 40-50 part fiber by dipping runner, obtains fiber impregnation material strip; Get 35-45 part poly(lactic acid), 25-35 part halogen-free flame retardants, 8-12 portions of synergist, 17-22 part char-forming agent, 1-3 part dispersion agent and 4-6 part compatilizer again and carry out drying, above-mentioned dried material is mixed with 0.4-0.6 part oxidation inhibitor, add in forcing machine after mixing of materials is even, when extruding, the mixture of melting is coated in fiber impregnation material strip, after cooling, pelletizing becomes the particle of 8 ~ 12 mm, obtains halogen-free flameproof long fiber reinforced Nylon 6 matrix material.
Described drying temperature is 60-80 DEG C, and time of drying is 5-8h.
In the present invention, flood runner and the mixture of melting be coated on the equipment that fiber impregnation material strip adopts, be the application number of applicant's earlier application for device disclosed in the application for a patent for invention of " 201110453139.8 ", namely realize the device that continuous roving glass fiber is extruded.
Owing to have employed technique scheme, compared with prior art, the present invention adopts nylon 6 as matrix resin, using SMA as compatilizer, this compatilizer enhances the bonding force between matrix resin and fiber, and adopt single stage method to prepare halogen-free flameproof long fiber reinforced Nylon 6 matrix material, the dipping of matrix resin to fiber is completed by impregnation mold by continuous print fiber, then complete in coating mould with halogen-free flame retardants matrix melt dipping material strip on coated, then cool, traction, desired length is cut into finally by dicing machine, compared with existing two-step approach, such mode not only technique is simple, and obtained product excellent in mechanical performance, environment-friendly type is good, and " floating fine " phenomenon easily occurred when solving glass fiber enhanced nylon.The present invention is simple, material source is extensive, with low cost, result of use is good.
Accompanying drawing explanation
Accompanying drawing 1 is schema of the present invention.
Embodiment
Embodiments of the invention 1: halogen-free flameproof long fiber reinforced Nylon 6 matrix material, calculate according to the mass fraction, comprise 90 parts of nylon, 6,45 parts of fibers, 10 parts of compatilizers, 1 part of oxidation inhibitor, 30 parts of halogen-free flame retardantss, 10 portions of synergist, 20 parts of char-forming agents and 2 parts of dispersion agents; Described fiber is glass fibre; Described compatilizer is styrene maleic anhydride copolymer; Described halogen-free flame retardants is aluminum phenylphosphinate; Described synergist is quaternary alkylphosphonium salt intercalated montmorillonite; Described Si modification phenolic aldehyde char-forming agent, described dispersion agent is tetramethylolmethane stearate.
The preparation method of halogen-free flameproof long fiber reinforced Nylon 6 matrix material, get 40 parts of poly(lactic acid) and 5 parts of compatilizer drying for standby respectively, above-mentioned dried poly(lactic acid) and compatilizer 0.5 part of oxidation inhibitor are mixed, then blending extrusion is carried out, processing temperature is 180 DEG C, melt is flooded 45 parts of fibers by dipping runner, obtains fiber impregnation material strip; Get 40 parts of poly(lactic acid) again, 30 parts of halogen-free flame retardantss, 10 portions of synergist, 20 parts of char-forming agents, 2 parts of dispersion agents and 5 parts of compatilizers carry out drying, above-mentioned dried material is mixed with 0.5 part of oxidation inhibitor, add in forcing machine after mixing of materials is even, when extruding, the mixture of melting is coated in fiber impregnation material strip, after cooling, pelletizing becomes the particle of 8 ~ 12 mm, obtains halogen-free flameproof long fiber reinforced Nylon 6 matrix material; Described drying temperature is 70 DEG C, and time of drying is 6h.
Embodiments of the invention 2: halogen-free flameproof long fiber reinforced Nylon 6 matrix material, calculate according to the mass fraction, comprise 80 parts of nylon, 6,50 parts of fibers, 12 parts of compatilizers, 0.8 part of oxidation inhibitor, 25 parts of halogen-free flame retardantss, 12 portions of synergist, 22 parts of char-forming agents and 1 part of dispersion agent; Described fiber is ramee; Described compatilizer is styrene maleic anhydride copolymer; Described halogen-free flame retardants is aluminum phenylphosphinate; Described synergist is quaternary alkylphosphonium salt intercalated montmorillonite; Described Si modification phenolic aldehyde char-forming agent, described dispersion agent is tetramethylolmethane stearate.
The preparation method of halogen-free flameproof long fiber reinforced Nylon 6 matrix material, get 45 parts of poly(lactic acid) and 6 parts of compatilizer drying for standby respectively, above-mentioned dried poly(lactic acid) and compatilizer 0.4 part of oxidation inhibitor are mixed, then blending extrusion is carried out, processing temperature is 150 DEG C, melt is flooded 50 parts of fibers by dipping runner, obtains fiber impregnation material strip; Get 35 parts of poly(lactic acid) again, 25 parts of halogen-free flame retardantss, 12 portions of synergist, 22 parts of char-forming agents, 1 part of dispersion agent and 6 parts of compatilizers carry out drying, above-mentioned dried material is mixed with 0.4 part of oxidation inhibitor, add in forcing machine after mixing of materials is even, when extruding, the mixture of melting is coated in fiber impregnation material strip, after cooling, pelletizing becomes the particle of 8 ~ 12 mm, obtains halogen-free flameproof long fiber reinforced Nylon 6 matrix material; Described drying temperature is 60 DEG C, and time of drying is 8h.
Embodiments of the invention 3: halogen-free flameproof long fiber reinforced Nylon 6 matrix material, calculate according to the mass fraction, comprise 100 parts of nylon, 6,40 parts of fibers, 8 parts of compatilizers, 1.2 parts of oxidation inhibitor, 35 parts of halogen-free flame retardantss, 8 portions of synergist, 17 parts of char-forming agents and 3 parts of dispersion agents; Described fiber is bamboo fibers; Described compatilizer is styrene maleic anhydride copolymer; Described halogen-free flame retardants is aluminum phenylphosphinate; Described synergist is quaternary alkylphosphonium salt intercalated montmorillonite; Described Si modification phenolic aldehyde char-forming agent, described dispersion agent is tetramethylolmethane stearate.
The preparation method of halogen-free flameproof long fiber reinforced Nylon 6 matrix material, get 55 parts of poly(lactic acid) and 4 parts of compatilizer drying for standby respectively, above-mentioned dried poly(lactic acid) and compatilizer 0.6 part of oxidation inhibitor are mixed, then blending extrusion is carried out, processing temperature is 200 DEG C, melt is flooded 40 parts of fibers by dipping runner, obtains fiber impregnation material strip; Get 45 parts of poly(lactic acid) again, 35 parts of halogen-free flame retardantss, 8 portions of synergist, 17 parts of char-forming agents, 3 parts of dispersion agents and 4 parts of compatilizers carry out drying, above-mentioned dried material is mixed with 0.6 part of oxidation inhibitor, add in forcing machine after mixing of materials is even, when extruding, the mixture of melting is coated in fiber impregnation material strip, after cooling, pelletizing becomes the particle of 8 ~ 12 mm, obtains halogen-free flameproof long fiber reinforced Nylon 6 matrix material; Described drying temperature is 80 DEG C, and time of drying is 5h.
In above-described embodiment, the trade mark of nylon 6 is 4042D; The trade mark of toughner is WB271; The trade mark of glass fibre is ER4301H; The trade mark of compatilizer is 1013B; The trade mark of oxidation inhibitor is AS4500; Oxidation inhibitor is 168 or 1098.
Salient features is tested: the product produced makes standard testing batten according to standard, carries out every test, and its performance test results is as shown in table 1.
Can learn according to table 1, adopt the preparation-obtained sample of technical scheme of the present invention, compared with the nylon 6 material of routine, its performance is good, and intensity is high, solves " floating fine " phenomenon of short fiber reinforced nylon 6 matrix material, and excellent fireproof performance.
Claims (8)
1. halogen-free flameproof long fiber reinforced Nylon 6 matrix material, it is characterized in that: calculate according to the mass fraction, comprise 80-100 part nylon 6,40-50 part fiber, 8-12 part compatilizer, 0.8-1.2 part oxidation inhibitor, 25-35 part halogen-free flame retardants, 8-12 portions of synergist, 17-22 part char-forming agent and 1-3 part dispersion agent.
2. halogen-free flameproof long fiber reinforced Nylon 6 matrix material according to claim 1, is characterized in that: described fiber is the arbitrary combination of one or more in ramee, jute fibre, flax fiber, hemp fibre, glass fibre, kenaf, sisal fibers or bamboo fibers.
3. halogen-free flameproof long fiber reinforced Nylon 6 matrix material according to claim 1, is characterized in that: described compatilizer is styrene maleic anhydride copolymer.
4. halogen-free flameproof long fiber reinforced Nylon 6 matrix material according to claim 1, is characterized in that: described halogen-free flame retardants is aluminum phenylphosphinate.
5. halogen-free flameproof long fiber reinforced Nylon 6 matrix material according to claim 1, is characterized in that: described synergist is quaternary alkylphosphonium salt intercalated montmorillonite.
6. halogen-free flameproof long fiber reinforced Nylon 6 matrix material according to claim 1, is characterized in that: described Si modification phenolic aldehyde char-forming agent, described dispersion agent is tetramethylolmethane stearate.
7. the preparation method of halogen-free flameproof long fiber reinforced Nylon 6 matrix material as claimed in claim 1, it is characterized in that: get 45-55 part poly(lactic acid) and 4-6 part compatilizer drying for standby respectively, above-mentioned dried poly(lactic acid) and compatilizer 0.4-0.6 part oxidation inhibitor are mixed, then blending extrusion is carried out, processing temperature is 150-200 DEG C, melt is flooded 40-50 part fiber by dipping runner, obtains fiber impregnation material strip; Get 35-45 part poly(lactic acid), 25-35 part halogen-free flame retardants, 8-12 portions of synergist, 17-22 part char-forming agent, 1-3 part dispersion agent and 4-6 part compatilizer again and carry out drying, above-mentioned dried material is mixed with 0.4-0.6 part oxidation inhibitor, add in forcing machine after mixing of materials is even, when extruding, the mixture of melting is coated in fiber impregnation material strip, after cooling, pelletizing becomes the particle of 8 ~ 12 mm, obtains halogen-free flameproof long fiber reinforced Nylon 6 matrix material.
8. the preparation method of high-performance halogen-free flame retardant long fiber reinforced Nylon 6 matrix material according to claim 7, it is characterized in that: described drying temperature is 60-80 DEG C, time of drying 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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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| CN114045043A (en) * | 2021-11-30 | 2022-02-15 | 浙江远景体育用品有限公司 | High-impact wood-plastic helmet composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| CN114045043A (en) * | 2021-11-30 | 2022-02-15 | 浙江远景体育用品有限公司 | High-impact wood-plastic helmet 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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