CN107226961A - A kind of modified flame-retardant polyamide/PP composite material - Google Patents
A kind of modified flame-retardant polyamide/PP composite material Download PDFInfo
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- CN107226961A CN107226961A CN201710583386.7A CN201710583386A CN107226961A CN 107226961 A CN107226961 A CN 107226961A CN 201710583386 A CN201710583386 A CN 201710583386A CN 107226961 A CN107226961 A CN 107226961A
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four 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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Abstract
The invention discloses a kind of modified flame-retardant polyamide/PP composite material, it is added to using nano modification stalk as fire-retardant filler in the preparation of polyamide/PP composite material.The present invention instead of poisonous and hazardous halogenated flame retardant using nano modification stalk, because nano modification stalk is to be dispersed in nano particle state in polyamide/PP composite material matrix, it can generate oxide and vapor when heat is decomposed, vapor, which waters down, dilutes imflammable gas, and the generation of oxide helps to make flameout, serve the effect for suppressing burning, generate protective layer and be covered in polymer body surface, isolate burning things which may cause a fire disaster and oxygen, therefore composite is made to be provided with good fire resistance, the present invention is effectively utilized agricultural wastes straw simultaneously, it is made to turn waste into wealth, create new application value.
Description
Technical field
The invention belongs to technical field of composite materials, more particularly to a kind of modified flame-retardant polyamide/PP composite material.
Background technology
Polyamide is commonly called as nylon (Nylon), English name Polyamide (PA), during it is macromolecular main chain repeat unit
The general name of high polymer containing amide group.Polyamide can be made by interior acid amide ring-opening polymerisation, also can be by diamine and binary acid
What polycondensation etc. was obtained.It is that DuPont develops resin for fiber at first, realizes and industrialize in nineteen thirty-nine.20th century
Start the fifties to develop and produce injection-molded item, the lightweight of downstream industry product is met with substituted metal, the requirement of cost is reduced.
PA has good combination property, including mechanical property, heat resistance, wear resistance, chemical proofing and self lubricity, and rubs
Wipe coefficient low, have certain anti-flammability, it is easy to process.
Polypropylene (PP), molecular formula (C3H6) n, be by propylene polymerization prepared by a kind of thermoplastic resin.Arranged by methyl
Column position is divided into isotactic polypropylene (isotaetic polyprolene), random polypropylene (atactic polypropylene)
With three kinds of syndiotactic polypropylene (syndiotatic polypropylene).Nontoxic, tasteless, density is small, and intensity, rigidity, hardness are resistance to
It is hot to be superior to low-pressure polyethylene, it can be used at 100 DEG C or so.With good electrical property and high-frequency insulation not by humidity shadow
Ring.Suitable for making common mechanical part, corrosion-resistant part and insulating part.The organic solvents such as common acid, alkali to it hardly
Work, available for tableware.
PA6/PP alloy materials combine the advantage of two kinds of materials.21 century electric appliance communication electromechanical equipment is to height
Performance miniaturization, to the requirement more and more higher of fire-retardant PP/PA6 alloy materials, meanwhile, with understanding of the mankind to environmental protection,
Green Product is by common concern.Therefore, the kind of the fire-retardant PP/PA6 alloy materials of environmental type can be more next with demand
It is more.And its conventional fire retardant is halogenated flame retardant at present, due to its efficient flame retardant effect, it is widely used in fire-retardant polymerization
During thing is material modified.But, the based flame retardant can discharge substantial amounts of poisonous and hazardous gas in burning, such as hydrogen halides,
The gases such as bioxin, cause secondary pollution, seriously endanger life security and Environmental security.
The content of the invention
It is an object of the invention to provide a kind of modification polyamides for not using halogenated flame retardant and having good fire resistance
Amine/PP composite material.
The purpose of the present invention can be achieved through the following technical solutions：
Modified polyamide/PP composite material of the present invention, is prepared using following methods step：
(1) dry stalk is crushed, stirring 1-2h is disperseed in water, filtering precipitate uses absolute ethyl alcohol and deionization again
Water supersound washing, filtering precipitate drying；
(2) stalk after step (1) is dried, which is crushed, to be added in the sodium hydroxide solution that mass fraction is 5-6%, in 50-
Filtering drying after 60 DEG C of immersion 5-6h；
(3) stalk after step (2) is dried is placed in Vaccum Permeating in the aluminum salt solution that concentration is 1.0-3.0molL-1
Note, then by the stalk after vacuum impregnation at 120-150 DEG C, the constant temperature 3-5h in hydrothermal reaction kettle is cooled to room temperature, takes out
Nano modification stalk is crushed to obtain in washing, vacuum drying；
(4) 60-75 parts of polyamides, 70-80 parts of acrylic resins, 5-8 parts of lubricants are weighed, high-speed mixer is added
In stir；
(5) 50-75 parts of nano modification stalks are weighed, be added in high-speed mixer stir, continuously add 10-15 parts it is compatible
Stir, take out standby in agent, 3-5 parts of antioxidant, mixer；
(6) step (5) resulting material is added in double screw extruder, in 220-260 DEG C of extruding pelletization.
It is preferred that modified flame-retardant polyamide/PP composite material described above, step (1) described stalk be Wheat Straw
Stalk.
It is preferred that modified flame-retardant polyamide/PP composite material described above, step (3) described aluminum salt solution be sulphur
Sour aluminum solutions, aluminum nitrate solution or liquor alumini chloridi.
It is preferred that modified flame-retardant polyamide/PP composite material described above, the processing of step (3) vacuum impregnation
Time is 5-8h, vacuum 0.1MPa.
It is preferred that modified flame-retardant polyamide/PP composite material described above, step (4) described polyamide is
PA6 resins.
It is preferred that modified flame-retardant polyamide/PP composite material described above, step (4) described lubricant is selected from hard
One or more in resin acid zinc, ethylene bis stearamide, erucyl amide, polypropylene wax, Tissuemat E, oleamide.
It is preferred that modified flame-retardant polyamide/PP composite material described above, step (5) described compatilizer be poly- third
Alkene grafted maleic anhydride.
It is preferred that modified flame-retardant polyamide/PP composite material described above, step (5) described antioxidant be antioxygen
Agent 1010 and irgasfos 168 in mass ratio 1:1 it is compound.
The present invention instead of poisonous and hazardous halogenated flame retardant using nano modification stalk, while the modified straw also may be used
As polymer-doped inorganic filler, so that nanometer stalk modified flame-retardant polyamide/PP composite material is made, wherein receiving
Rice modified straw is the nano-aluminum hydroxide modified straw by generation, because nano modification stalk is with nano particle state point
It is dispersed in resin matrix, it can generate oxide and vapor when heat is decomposed, vapor, which waters down, dilutes imflammable gas,
And the generation of oxide helps to make flameout, the effect for suppressing burning is served, protective layer is generated and is covered in polymer
Body surface, isolation burning things which may cause a fire disaster and oxygen, therefore composite is provided with good fire resistance, using the fire-protection ratings of UL 94
Test, gained resin material fire-retardant fireproof grade reaches V-0.Stalk is widely present in China simultaneously, can all be produced every year a large amount of
Stalk, be a kind of behave turned waste into wealth in polymer-modified application stalk, on the one hand can give increasing peasant income, on the other hand
The burning pollution on the environment of stalk can be reduced.The present invention is effectively utilized agricultural wastes straw, make its change give up into
Treasured, creates new application value.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples agents useful for same is only for example
Protection domain that is bright, being not intended to limit the invention, other embodiments of the invention still elect to all in right
Optional reagent.Unless otherwise instructed, the number is mass parts.
Embodiment 1
(1) dry wheat stalk is crushed, disperses stirring 2h in water, filtering precipitate again with absolute ethyl alcohol and go from
Sub- water supersound washing, filtering precipitate drying；
(2) stalk after step (1) is dried, which is crushed, to be added in the sodium hydroxide solution that mass fraction is 6%, at 50 DEG C
Soak filtering drying after 6h；
(3) stalk after step (2) is dried is placed in vacuum impregnation in the aluminum nitrate solution that concentration is 3.0molL-1,
Then by the stalk after vacuum impregnation at 120 DEG C, the constant temperature 5h in hydrothermal reaction kettle is cooled to room temperature, takes out washing, vacuum
Drying and crushing obtains nano modification stalk；Vacuum impregnation processing time is 5h, vacuum 0.1MPa；
(4) 60 parts of PA6 resins, 70 parts of acrylic resins, 5 parts of lubricant polyethylene waxes are weighed, are added in high-speed mixer
Stir；
(5) 50 parts of nano modification stalks are weighed, is added in high-speed mixer and stirs, continuously add 10 parts of compatilizers poly- third
Alkene grafted maleic anhydride, 3 parts of antioxidant (antioxidant 1010 and irgasfos 168s in mass ratio 1:1 it is compound), stir in mixer
Mix, take out standby；
(6) step (5) resulting material is added in double screw extruder, in 220-260 DEG C of extruding pelletization.Using UL 94
Fire-protection rating is tested, and gained modified flame-retardant polyamide/PP composite material fire-retardant fireproof grade reaches V-0.
Embodiment 2
(1) dry wheat stalk is crushed, disperses stirring 2h in water, filtering precipitate again with absolute ethyl alcohol and go from
Sub- water supersound washing, filtering precipitate drying；
(2) stalk after step (1) is dried, which is crushed, to be added in the sodium hydroxide solution that mass fraction is 5%, at 50 DEG C
Soak filtering drying after 5h；
(3) stalk after step (2) is dried is placed in vacuum impregnation in the aluminum nitrate solution that concentration is 1.0molL-1,
Then by the stalk after vacuum impregnation at 150 DEG C, the constant temperature 3h in hydrothermal reaction kettle is cooled to room temperature, takes out washing, vacuum
Drying and crushing obtains nano modification stalk；Vacuum impregnation processing time is 8h, vacuum 0.1MPa；
(4) 65 parts of PA6 resins, 75 parts of acrylic resins, 6 parts of lubricant polyethylene waxes are weighed, are added in high-speed mixer
Stir；
(5) 50 parts of nano modification stalks are weighed, is added in high-speed mixer and stirs, continuously add 12 parts of compatilizers poly- third
Alkene grafted maleic anhydride, 3 parts of antioxidant (antioxidant 1010 and irgasfos 168s in mass ratio 1:1 it is compound), stir in mixer
Mix, take out standby；
(6) step (5) resulting material is added in double screw extruder, in 220-260 DEG C of extruding pelletization.Using UL 94
Fire-protection rating is tested, and gained modified flame-retardant polyamide/PP composite material fire-retardant fireproof grade reaches V-0.
Embodiment 3
(1) dry wheat stalk is crushed, disperses stirring 1h in water, filtering precipitate again with absolute ethyl alcohol and go from
Sub- water supersound washing, filtering precipitate drying；
(2) stalk after step (1) is dried, which is crushed, to be added in the sodium hydroxide solution that mass fraction is 5%, at 50 DEG C
Soak filtering drying after 5h；
(3) stalk after step (2) is dried is placed in vacuum impregnation in the aluminum nitrate solution that concentration is 1.0molL-1,
Then by the stalk after vacuum impregnation at 120 DEG C, the constant temperature 5h in hydrothermal reaction kettle is cooled to room temperature, takes out washing, vacuum
Drying and crushing obtains nano modification stalk；Vacuum impregnation processing time is 8h, vacuum 0.1MPa；
(4) 70 parts of PA6 resins, 80 parts of acrylic resins, 7 parts of lubricant polyethylene waxes are weighed, are added in high-speed mixer
Stir；
(5) 75 parts of nano modification stalks are weighed, is added in high-speed mixer and stirs, continuously add 15 parts of compatilizers poly- third
Alkene grafted maleic anhydride, 4 parts of antioxidant (antioxidant 1010 and irgasfos 168s in mass ratio 1:1 it is compound), stir in mixer
Mix, take out standby；
(6) step (5) resulting material is added in double screw extruder, in 220-260 DEG C of extruding pelletization.Using UL 94
Fire-protection rating is tested, and gained modified flame-retardant polyamide/PP composite material fire-retardant fireproof grade reaches V-0.
Embodiment 4
(1) dry wheat stalk is crushed, disperses stirring 1h in water, filtering precipitate again with absolute ethyl alcohol and go from
Sub- water supersound washing, filtering precipitate drying；
(2) stalk after step (1) is dried, which is crushed, to be added in the sodium hydroxide solution that mass fraction is 5%, at 60 DEG C
Soak filtering drying after 5h；
(3) stalk after step (2) is dried is placed in vacuum impregnation in the aluminum nitrate solution that concentration is 3.0molL-1,
Then by the stalk after vacuum impregnation at 150 DEG C, the constant temperature 3h in hydrothermal reaction kettle is cooled to room temperature, takes out washing, vacuum
Drying and crushing obtains nano modification stalk；Vacuum impregnation processing time is 5h, vacuum 0.1MPa；
(4) 75 parts of PA6 resins, 80 parts of acrylic resins, 6 parts of lubricant polyethylene waxes are weighed, are added in high-speed mixer
Stir；
(5) 70 parts of nano modification stalks are weighed, is added in high-speed mixer and stirs, continuously add 10 parts of compatilizers poly- third
Alkene grafted maleic anhydride, 4 parts of antioxidant (antioxidant 1010 and irgasfos 168s in mass ratio 1:1 it is compound), stir in mixer
Mix, take out standby；
(6) step (5) resulting material is added in double screw extruder, in 220-260 DEG C of extruding pelletization.Using UL 94
Fire-protection rating is tested, and gained modified flame-retardant polyamide/PP composite material fire-retardant fireproof grade reaches V-0.
Embodiment 5
(1) dry wheat stalk is crushed, disperses stirring 2h in water, filtering precipitate again with absolute ethyl alcohol and go from
Sub- water supersound washing, filtering precipitate drying；
(2) stalk after step (1) is dried, which is crushed, to be added in the sodium hydroxide solution that mass fraction is 5%, at 50 DEG C
Soak filtering drying after 6h；
(3) stalk after step (2) is dried is placed in vacuum impregnation in the aluminum nitrate solution that concentration is 1.0molL-1,
Then by the stalk after vacuum impregnation at 120 DEG C, the constant temperature 3h in hydrothermal reaction kettle is cooled to room temperature, takes out washing, vacuum
Drying and crushing obtains nano modification stalk；Vacuum impregnation processing time is 8h, vacuum 0.1MPa；
(4) 65 parts of PA6 resins, 75 parts of acrylic resins, 5 parts of lubricant polyethylene waxes are weighed, are added in high-speed mixer
Stir；
(5) 50-75 parts of nano modification stalks are weighed, is added in high-speed mixer and stirs, continuously add 10 parts of compatilizers
Polypropylene grafted maleic anhydride, 3 parts of antioxidant (antioxidant 1010 and irgasfos 168s in mass ratio 1:1 it is compound), in mixer
Stirring, takes out standby；
(6) step (5) resulting material is added in double screw extruder, in 220-260 DEG C of extruding pelletization.Using UL 94
Fire-protection rating is tested, and gained modified flame-retardant polyamide/PP composite material fire-retardant fireproof grade reaches V-0.
Embodiment 6
(1) dry wheat stalk is crushed, disperses stirring 1h in water, filtering precipitate again with absolute ethyl alcohol and go from
Sub- water supersound washing, filtering precipitate drying；
(2) stalk after step (1) is dried, which is crushed, to be added in the sodium hydroxide solution that mass fraction is 5%, at 50 DEG C
Soak filtering drying after 5h；
(3) stalk after step (2) is dried is placed in vacuum impregnation in the aluminum nitrate solution that concentration is 2.0molL-1,
Then by the stalk after vacuum impregnation at 140 DEG C, the constant temperature 5h in hydrothermal reaction kettle is cooled to room temperature, takes out washing, vacuum
Drying and crushing obtains nano modification stalk；Vacuum impregnation processing time is 6h, vacuum 0.1MPa；
(4) 60 parts of PA6 resins, 80 parts of acrylic resins, 6 parts of lubricant polyethylene waxes are weighed, are added in high-speed mixer
Stir；
(5) 75 parts of nano modification stalks are weighed, is added in high-speed mixer and stirs, continuously add 12 parts of compatilizers poly- third
Alkene grafted maleic anhydride, 4 parts of antioxidant (antioxidant 1010 and irgasfos 168s in mass ratio 1:1 it is compound), stir in mixer
Mix, take out standby；
(6) step (5) resulting material is added in double screw extruder, in 220-260 DEG C of extruding pelletization.Using UL 94
Fire-protection rating is tested, and gained modified flame-retardant polyamide/PP composite material fire-retardant fireproof grade reaches V-0.
Claims (8)
1. a kind of modified flame-retardant polyamide/PP composite material, it is characterised in that prepared using following methods step：
(1) dry stalk is crushed, stirring 1-2h is disperseed in water, filtering precipitate is super with absolute ethyl alcohol and deionized water again
Sound is washed, filtering precipitate drying；
(2) stalk after step (1) is dried, which is crushed, to be added in the sodium hydroxide solution that mass fraction is 5-6%, at 50-60 DEG C
Soak filtering drying after 5-6h；
(3) stalk after step (2) is dried is placed in vacuum impregnation in the aluminum salt solution that concentration is 1.0-3.0molL-1, so
Afterwards by the stalk after vacuum impregnation at 120-150 DEG C, the constant temperature 3-5h in hydrothermal reaction kettle is cooled to room temperature, takes out washing,
Nano modification stalk is crushed to obtain in vacuum drying；
(4) 60-75 parts of polyamides, 70-80 parts of acrylic resins, 5-8 parts of lubricants are weighed, adds and is stirred in high-speed mixer
Mix uniform；
(5) 50-75 parts of nano modification stalks are weighed, be added in high-speed mixer stir, continuously add 10-15 parts of compatilizers,
Stir, take out standby in 3-5 parts of antioxidant, mixer；
(6) step (5) resulting material is added in double screw extruder, in 220-260 DEG C of extruding pelletization.
2. modified flame-retardant polyamide/PP composite material as claimed in claim 1, it is characterised in that step (1) described straw
Stalk is wheat stalk.
3. modified flame-retardant polyamide/PP composite material as claimed in claim 1, it is characterised in that step (3) described aluminium
Salting liquid is aluminum sulfate solution, aluminum nitrate solution or liquor alumini chloridi.
4. modified flame-retardant polyamide/PP composite material as claimed in claim 1, it is characterised in that step (3) is described true
The empty Immersion treatment time is 5-8h, vacuum 0.1MPa.
5. modified flame-retardant polyamide/PP composite material as claimed in claim 1, it is characterised in that step (4) is described poly-
Amide resin is PA6 resins.
6. modified flame-retardant polyamide/PP composite material as claimed in claim 1, it is characterised in that step (4) profit
One kind in zinc stearate, ethylene bis stearamide, erucyl amide, polypropylene wax, Tissuemat E, oleamide of lubrication prescription or
It is several.
7. modified flame-retardant polyamide/PP composite material as claimed in claim 1, it is characterised in that step (5) described phase
Appearance agent is polypropylene grafted maleic anhydride.
8. modified flame-retardant polyamide/PP composite material as claimed in claim 1, it is characterised in that step (5) is described anti-
Oxygen agent is antioxidant 1010 and irgasfos 168 in mass ratio 1:1 it is compound.
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| CN104356511A (en) * | 2014-11-26 | 2015-02-18 | 朱建一 | High-rigidity creep-resistant long-fiber-reinforced master batch for wood plastic products, and preparation and mold thereof |
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